# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1419429'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

#end of refcif 
_cell_length_a                   20.1905(14)
_cell_length_b                   6.830(2)
_cell_length_c                   9.5946(7)
_cell_angle_alpha                90
_cell_angle_beta                 112.981(4)
_cell_angle_gamma                90
_cell_volume                     1218.0(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.85 Fooo =    696.00 Mu =      7.37 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.85 FOOO =    696.00 Mu =      7.37 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.737

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4725
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         340
_diffrn_reflns_number            4189
_reflns_number_total             1044
_diffrn_reflns_av_R_equivalents  0.046
# Number of reflections without Friedels Law is 1044 
# Number of reflections with Friedels Law is 652 
# Theoretical number of reflections is about 1245 


_diffrn_reflns_theta_min         1.576
_diffrn_reflns_theta_max         17.677
_diffrn_measured_fraction_theta_max 0.480

_diffrn_reflns_theta_full        13.964
_diffrn_measured_fraction_theta_full 0.492


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -25
_reflns_limit_h_max              23
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.58
_refine_diff_density_max         0.55


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         1035
_refine_ls_number_restraints     171
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0510
_refine_ls_wR_factor_ref         0.0639
_refine_ls_goodness_of_fit_ref   0.9888
_refine_ls_shift/su_max          0.0003859
_refine_ls_shift/su_mean         0.0000604


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1035
_refine_ls_R_factor_all          0.0510
_refine_ls_wR_factor_all         0.0639

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                949
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_gt          0.0631

_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_abs_structure_details 'Flack (1983), 392 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8048(4) 0.0000 0.0254 1.0000 Uani S T . . . .
Na1 Na 0.73787(8) 0.5512(9) 0.49197(19) 0.0309 1.0000 Uani . . . . . .
Na2 Na 0.52351(7) 0.4920(7) 0.28234(14) 0.0310 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0232(10) 0.5000 0.0445 1.0000 Uani S T . . . .
C1 C 0.35304(14) 0.8328(17) -0.2086(3) 0.0286 1.0000 Uani D U . . . .
O11 O 0.28984(10) 0.8045(15) -0.3000(2) 0.0373 1.0000 Uani D U . . . .
O12 O 0.40854(10) 0.8085(16) -0.2395(2) 0.0281 1.0000 Uani D U . . . .
C2 C 0.36795(15) 0.8885(11) -0.0433(4) 0.0283 1.0000 Uani D U . . . .
O21 O 0.43436(11) 0.9892(12) 0.0202(3) 0.0303 1.0000 Uani D U . . . .
C3 C 0.37853(15) 0.6992(11) 0.0465(4) 0.0293 1.0000 Uani D U . . . .
O31 O 0.44292(12) 0.6122(12) 0.0491(3) 0.0301 1.0000 Uani D U . . . .
C4 C 0.38198(17) 0.7465(15) 0.2081(3) 0.0277 1.0000 Uani D U . . . .
O41 O 0.43579(13) 0.6948(12) 0.3209(3) 0.0331 1.0000 Uani D U . . . .
O42 O 0.32769(12) 0.8255(15) 0.2133(3) 0.0509 1.0000 Uani D U . . . .
O1 O 0.81044(14) 0.7717(18) 0.1602(3) 0.0494 1.0000 Uani . U . . . .
O2 O 0.58171(11) 0.3230(15) 0.1451(3) 0.0325 1.0000 Uani . U . . . .
O3 O 0.62474(13) 0.4573(14) 0.5070(3) 0.0323 1.0000 Uani . U . . . .
O4 O 0.45926(13) 0.1942(13) 0.2869(3) 0.0354 1.0000 Uani . U . . . .
O5 O 0.72204(10) 0.2953(16) 0.3235(2) 0.0371 1.0000 Uani . U . . . .
O6 O 0.87299(14) 0.5273(15) 0.4926(3) 0.0342 1.0000 Uani . U . . . .
H2 H 0.3277 0.9666 -0.0366 0.0355 1.0000 Uiso . . . . . .
H3 H 0.3375 0.6081 -0.0061 0.0367 1.0000 Uiso . . . . . .
H11 H 0.7811 0.7841 0.2026 0.0738 1.0000 Uiso . . . . . .
H12 H 0.8155 0.6540 0.1757 0.0738 1.0000 Uiso . . . . . .
H21 H 0.5768 0.2195 0.0946 0.0486 1.0000 Uiso . . . . . .
H22 H 0.5739 0.4146 0.0837 0.0486 1.0000 Uiso . . . . . .
H31 H 0.6251 0.3344 0.5058 0.0504 1.0000 Uiso . . . . . .
H32 H 0.6069 0.5257 0.5554 0.0504 1.0000 Uiso . . . . . .
H41 H 0.4517 0.1328 0.2064 0.0539 1.0000 Uiso . . . . . .
H42 H 0.4149 0.2189 0.2494 0.0539 1.0000 Uiso . . . . . .
H51 H 0.6781 0.3028 0.2679 0.0548 1.0000 Uiso . . . . . .
H52 H 0.7545 0.3038 0.2897 0.0548 1.0000 Uiso . . . . . .
H61 H 0.8594 0.4670 0.4096 0.0502 1.0000 Uiso . . . . . .
H62 H 0.8835 0.4618 0.5730 0.0502 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2753(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.319(2) yes
Mn1 . O31 3_655 1.924(6) yes
Mn1 . O21 3_655 1.892(7) yes
Mn1 . O12 . 2.319(2) yes
Mn1 . O21 . 1.892(7) yes
Mn1 . O31 . 1.924(6) yes
Na1 . O5 4_656 2.335(10) yes
Na1 . O11 3_655 2.428(9) yes
Na1 . O11 2_546 2.508(9) yes
Na1 . O3 . 2.430(4) yes
Na1 . O5 . 2.317(10) yes
Na1 . O6 . 2.731(3) yes
Na2 . O12 3_655 2.677(10) yes
Na2 . O31 . 2.342(4) yes
Na2 . O41 . 2.388(6) yes
Na2 . O2 . 2.378(6) yes
Na2 . O3 . 2.332(3) yes
Na2 . O4 . 2.422(9) yes
Na3 . O4 3_656 2.397(8) yes
Na3 . O6 2_445 2.561(3) yes
Na3 . O6 4_646 2.561(3) yes
Na3 . O41 1_545 2.569(9) yes
Na3 . O41 3_646 2.569(9) yes
Na3 . O4 . 2.397(8) yes
C1 . O11 . 1.249(4) yes
C1 . O12 . 1.277(4) yes
C1 . C2 . 1.541(5) yes
C2 . O21 . 1.416(6) yes
C2 . C3 . 1.522(7) yes
C2 . H2 . 0.995 no
C3 . O31 . 1.421(5) yes
C3 . C4 . 1.559(4) yes
C3 . H3 . 1.001 no
C4 . O41 . 1.248(5) yes
C4 . O42 . 1.240(6) yes
O1 . H11 . 0.844 no
O1 . H12 . 0.817 no
O2 . H21 . 0.841 no
O2 . H22 . 0.831 no
O3 . H31 . 0.839 no
O3 . H32 . 0.834 no
O4 . H41 . 0.839 no
O4 . H42 . 0.842 no
O5 . H51 . 0.840 no
O5 . H52 . 0.838 no
O6 . H61 . 0.842 no
O6 . H62 . 0.843 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 85.9(2) yes
O12 3_655 Mn1 . O21 3_655 77.0(2) yes
O31 3_655 Mn1 . O21 3_655 85.4(2) yes
O12 3_655 Mn1 . O12 . 178.7(6) yes
O31 3_655 Mn1 . O12 . 95.0(2) yes
O21 3_655 Mn1 . O12 . 102.1(2) yes
O12 3_655 Mn1 . O21 . 102.1(2) yes
O31 3_655 Mn1 . O21 . 171.99(12) yes
O21 3_655 Mn1 . O21 . 96.6(4) yes
O12 . Mn1 . O21 . 77.0(2) yes
O12 3_655 Mn1 . O31 . 95.0(2) yes
O31 3_655 Mn1 . O31 . 93.8(4) yes
O21 3_655 Mn1 . O31 . 171.99(12) yes
O12 . Mn1 . O31 . 85.9(2) yes
O21 . Mn1 . O31 . 85.4(2) yes
O5 4_656 Na1 . O11 3_655 88.6(4) yes
O5 4_656 Na1 . O11 2_546 87.9(2) yes
O11 3_655 Na1 . O11 2_546 169.59(15) yes
O5 4_656 Na1 . O3 . 101.5(2) yes
O11 3_655 Na1 . O3 . 106.8(2) yes
O11 2_546 Na1 . O3 . 83.5(2) yes
O5 4_656 Na1 . O5 . 168.66(15) yes
O11 3_655 Na1 . O5 . 94.6(2) yes
O11 2_546 Na1 . O5 . 87.1(4) yes
O3 . Na1 . O5 . 88.0(2) yes
O5 4_656 Na1 . O6 . 89.5(2) yes
O11 3_655 Na1 . O6 . 88.8(2) yes
O11 2_546 Na1 . O6 . 81.42(19) yes
O3 . Na1 . O6 . 161.0(5) yes
O5 . Na1 . O6 . 79.7(2) yes
O12 3_655 Na2 . O31 . 77.1(2) yes
O12 3_655 Na2 . O41 . 90.6(3) yes
O31 . Na2 . O41 . 70.40(16) yes
O12 3_655 Na2 . O2 . 85.0(3) yes
O31 . Na2 . O2 . 87.15(17) yes
O41 . Na2 . O2 . 157.52(14) yes
O12 3_655 Na2 . O3 . 84.7(2) yes
O31 . Na2 . O3 . 161.8(3) yes
O41 . Na2 . O3 . 110.56(19) yes
O2 . Na2 . O3 . 91.03(16) yes
O12 3_655 Na2 . O4 . 172.42(13) yes
O31 . Na2 . O4 . 97.7(2) yes
O41 . Na2 . O4 . 92.8(2) yes
O2 . Na2 . O4 . 89.2(3) yes
O3 . Na2 . O4 . 100.4(3) yes
O4 3_656 Na3 . O6 2_445 86.9(2) yes
O4 3_656 Na3 . O6 4_646 83.5(2) yes
O6 2_445 Na3 . O6 4_646 164.5(6) yes
O4 3_656 Na3 . O41 1_545 161.8(2) yes
O6 2_445 Na3 . O41 1_545 81.0(2) yes
O6 4_646 Na3 . O41 1_545 111.0(2) yes
O4 3_656 Na3 . O41 3_646 88.76(19) yes
O6 2_445 Na3 . O41 3_646 111.0(2) yes
O6 4_646 Na3 . O41 3_646 81.0(2) yes
O41 1_545 Na3 . O41 3_646 82.9(3) yes
O4 3_656 Na3 . O4 . 103.5(4) yes
O6 2_445 Na3 . O4 . 83.5(2) yes
O6 4_646 Na3 . O4 . 86.9(2) yes
O41 1_545 Na3 . O4 . 88.76(19) yes
O41 3_646 Na3 . O4 . 161.8(2) yes
O11 . C1 . O12 . 124.4(4) yes
O11 . C1 . C2 . 119.7(2) yes
O12 . C1 . C2 . 115.7(2) yes
Na1 3_655 O11 . Na1 2_454 88.50(7) yes
Na1 3_655 O11 . C1 . 120.8(6) yes
Na1 2_454 O11 . C1 . 116.7(7) yes
Mn1 . O12 . C1 . 101.70(17) yes
Mn1 . O12 . Na2 3_655 83.4(2) yes
C1 . O12 . Na2 3_655 133.6(7) yes
C1 . C2 . O21 . 109.6(3) yes
C1 . C2 . C3 . 107.5(5) yes
O21 . C2 . C3 . 105.6(4) yes
C1 . C2 . H2 . 111.2 no
O21 . C2 . H2 . 111.9 no
C3 . C2 . H2 . 110.9 no
C2 . O21 . Mn1 . 102.5(5) yes
C2 . C3 . O31 . 106.9(4) yes
C2 . C3 . C4 . 109.2(5) yes
O31 . C3 . C4 . 112.6(3) yes
C2 . C3 . H3 . 109.7 no
O31 . C3 . H3 . 108.7 no
C4 . C3 . H3 . 109.6 no
Na2 . O31 . C3 . 116.91(19) yes
Na2 . O31 . Mn1 . 102.37(15) yes
C3 . O31 . Mn1 . 109.9(5) yes
C3 . C4 . O41 . 119.3(4) yes
C3 . C4 . O42 . 115.7(3) yes
O41 . C4 . O42 . 124.9(3) yes
Na2 . O41 . Na3 1_565 109.10(14) yes
Na2 . O41 . C4 . 118.5(3) yes
Na3 1_565 O41 . C4 . 114.1(7) yes
H11 . O1 . H12 . 94.1 no
Na2 . O2 . H21 . 139.1 no
Na2 . O2 . H22 . 91.7 no
H21 . O2 . H22 . 106.0 no
Na2 . O3 . Na1 . 115.04(19) yes
Na2 . O3 . H31 . 95.7 no
Na1 . O3 . H31 . 104.4 no
Na2 . O3 . H32 . 92.5 no
Na1 . O3 . H32 . 120.4 no
H31 . O3 . H32 . 125.2 no
Na3 . O4 . Na2 . 121.86(17) yes
Na3 . O4 . H41 . 110.8 no
Na2 . O4 . H41 . 108.0 no
Na3 . O4 . H42 . 116.3 no
Na2 . O4 . H42 . 108.2 no
H41 . O4 . H42 . 85.7 no
Na1 . O5 . Na1 4_646 95.55(8) yes
Na1 . O5 . H51 . 102.7 no
Na1 4_646 O5 . H51 . 119.5 no
Na1 . O5 . H52 . 107.6 no
Na1 4_646 O5 . H52 . 104.5 no
H51 . O5 . H52 . 122.8 no
Na3 2_555 O6 . Na1 . 175.5(5) yes
Na3 2_555 O6 . H61 . 85.0 no
Na1 . O6 . H61 . 94.1 no
Na3 2_555 O6 . H62 . 90.6 no
Na1 . O6 . H62 . 85.9 no
H61 . O6 . H62 . 118.5 no


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1419430'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_2                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_2                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_2                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_2                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_2                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_2                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_2                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

#end of refcif 
_cell_length_a                   20.1241(14)
_cell_length_b                   6.800(2)
_cell_length_c                   9.5772(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.069(4)
_cell_angle_gamma                90
_cell_volume                     1205.8(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.87 Fooo =    696.00 Mu =      7.45 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.87 FOOO =    696.00 Mu =      7.45 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.745

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4719
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            4356
_reflns_number_total             1130
_diffrn_reflns_av_R_equivalents  0.051
# Number of reflections without Friedels Law is 1130 
# Number of reflections with Friedels Law is 699 
# Theoretical number of reflections is about 1332 


_diffrn_reflns_theta_min         1.492
_diffrn_reflns_theta_max         17.115
_diffrn_measured_fraction_theta_max 0.481

_diffrn_reflns_theta_full        12.836
_diffrn_measured_fraction_theta_full 0.499


_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -25
_reflns_limit_h_max              23
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.63
_refine_diff_density_max         0.58


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         1115
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0495
_refine_ls_wR_factor_ref         0.1035
_refine_ls_goodness_of_fit_ref   1.0190
_refine_ls_shift/su_max          0.0005314
_refine_ls_shift/su_mean         0.0000525


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1115
_refine_ls_R_factor_all          0.0495
_refine_ls_wR_factor_all         0.1035

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1015
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_gt          0.0926

_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_abs_structure_details 'Flack (1983), 431 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 6.31 7.78 2.33 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8058(5) 0.0000 0.0308 1.0000 Uani S T . . . .
Na1 Na 0.73792(13) 0.5493(11) 0.4921(3) 0.0373 1.0000 Uani . . . . . .
Na2 Na 0.52327(12) 0.4913(9) 0.2832(2) 0.0345 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0243(14) 0.5000 0.0437 1.0000 Uani S T . . . .
C1 C 0.3525(2) 0.833(3) -0.2094(5) 0.0307 1.0000 Uani . U . . . .
O11 O 0.28935(18) 0.8066(19) -0.3014(4) 0.0396 1.0000 Uani . U . . . .
O12 O 0.40858(17) 0.814(2) -0.2395(4) 0.0322 1.0000 Uani . U . . . .
C2 C 0.3673(3) 0.889(2) -0.0442(5) 0.0291 1.0000 Uani . U . . . .
O21 O 0.4341(2) 0.9907(17) 0.0196(4) 0.0316 1.0000 Uani . U . . . .
C3 C 0.3779(3) 0.7001(19) 0.0462(6) 0.0289 1.0000 Uani . U . . . .
O31 O 0.4427(2) 0.6127(16) 0.0497(4) 0.0310 1.0000 Uani . U . . . .
C4 C 0.3811(3) 0.743(2) 0.2069(6) 0.0306 1.0000 Uani . U . . . .
O41 O 0.4354(2) 0.6930(15) 0.3206(4) 0.0353 1.0000 Uani . U . . . .
O42 O 0.3264(2) 0.825(2) 0.2122(5) 0.0442 1.0000 Uani . U . . . .
O1 O 0.8104(2) 0.778(3) 0.1588(6) 0.0705 1.0000 Uani . . . . . .
O2 O 0.58115(18) 0.3184(19) 0.1454(4) 0.0346 1.0000 Uani . U . . . .
O3 O 0.6251(2) 0.4583(17) 0.5076(5) 0.0373 1.0000 Uani . U . . . .
O4 O 0.4588(2) 0.1975(17) 0.2871(5) 0.0382 1.0000 Uani . U . . . .
O5 O 0.72150(18) 0.288(2) 0.3236(4) 0.0405 1.0000 Uani . U . . . .
O6 O 0.8726(3) 0.5255(18) 0.4917(5) 0.0358 1.0000 Uani . U . . . .
H2 H 0.3271 0.9701 -0.0377 0.0355 1.0000 Uiso . . . . . .
H3 H 0.3367 0.6088 -0.0075 0.0352 1.0000 Uiso . . . . . .
H11 H 0.7812 0.7884 0.2019 0.1062 1.0000 Uiso . . . . . .
H12 H 0.8150 0.6583 0.1741 0.1062 1.0000 Uiso . . . . . .
H21 H 0.5764 0.2156 0.0943 0.0521 1.0000 Uiso . . . . . .
H22 H 0.5736 0.4113 0.0841 0.0521 1.0000 Uiso . . . . . .
H31 H 0.6257 0.3348 0.5069 0.0578 1.0000 Uiso . . . . . .
H32 H 0.6075 0.5266 0.5567 0.0578 1.0000 Uiso . . . . . .
H41 H 0.4514 0.1355 0.2066 0.0576 1.0000 Uiso . . . . . .
H42 H 0.4144 0.2229 0.2489 0.0576 1.0000 Uiso . . . . . .
H51 H 0.6774 0.2977 0.2679 0.0613 1.0000 Uiso . . . . . .
H52 H 0.7538 0.2998 0.2893 0.0613 1.0000 Uiso . . . . . .
H61 H 0.8588 0.4646 0.4083 0.0522 1.0000 Uiso . . . . . .
H62 H 0.8835 0.4605 0.5731 0.0522 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2776(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.311(3) yes
Mn1 . O31 3_655 1.926(8) yes
Mn1 . O21 3_655 1.890(8) yes
Mn1 . O12 . 2.311(3) yes
Mn1 . O21 . 1.890(8) yes
Mn1 . O31 . 1.926(8) yes
Na1 . O5 4_656 2.302(12) yes
Na1 . O11 3_655 2.432(11) yes
Na1 . O11 2_546 2.470(11) yes
Na1 . O3 . 2.412(6) yes
Na1 . O5 . 2.333(12) yes
Na1 . O6 . 2.717(5) yes
Na2 . O12 3_655 2.706(12) yes
Na2 . O31 . 2.339(6) yes
Na2 . O41 . 2.373(8) yes
Na2 . O2 . 2.384(8) yes
Na2 . O3 . 2.327(5) yes
Na2 . O4 . 2.390(12) yes
Na3 . O4 3_656 2.407(10) yes
Na3 . O6 4_646 2.556(5) yes
Na3 . O6 2_445 2.556(5) yes
Na3 . O41 1_545 2.566(11) yes
Na3 . O41 3_646 2.566(11) yes
Na3 . O4 . 2.407(10) yes
C1 . O11 . 1.243(6) yes
C1 . O12 . 1.276(6) yes
C1 . C2 . 1.539(8) yes
C2 . O21 . 1.419(10) yes
C2 . C3 . 1.516(18) yes
C2 . H2 . 1.002 no
C3 . O31 . 1.421(9) yes
C3 . C4 . 1.543(8) yes
C3 . H3 . 1.003 no
C4 . O41 . 1.251(8) yes
C4 . O42 . 1.252(11) yes
O1 . H11 . 0.843 no
O1 . H12 . 0.825 no
O2 . H21 . 0.837 no
O2 . H22 . 0.836 no
O3 . H31 . 0.840 no
O3 . H32 . 0.833 no
O4 . H41 . 0.839 no
O4 . H42 . 0.841 no
O5 . H51 . 0.839 no
O5 . H52 . 0.839 no
O6 . H61 . 0.845 no
O6 . H62 . 0.847 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.6(3) yes
O12 3_655 Mn1 . O21 3_655 76.5(3) yes
O31 3_655 Mn1 . O21 3_655 85.3(3) yes
O12 3_655 Mn1 . O12 . 177.3(7) yes
O31 3_655 Mn1 . O12 . 95.3(3) yes
O21 3_655 Mn1 . O12 . 101.7(3) yes
O12 3_655 Mn1 . O21 . 101.7(3) yes
O31 3_655 Mn1 . O21 . 171.72(17) yes
O21 3_655 Mn1 . O21 . 96.6(6) yes
O12 . Mn1 . O21 . 76.5(3) yes
O12 3_655 Mn1 . O31 . 95.3(3) yes
O31 3_655 Mn1 . O31 . 94.0(5) yes
O21 3_655 Mn1 . O31 . 171.72(17) yes
O12 . Mn1 . O31 . 86.6(3) yes
O21 . Mn1 . O31 . 85.3(3) yes
O5 4_656 Na1 . O11 3_655 88.6(4) yes
O5 4_656 Na1 . O11 2_546 87.0(3) yes
O11 3_655 Na1 . O11 2_546 169.3(2) yes
O5 4_656 Na1 . O3 . 101.2(3) yes
O11 3_655 Na1 . O3 . 106.8(3) yes
O11 2_546 Na1 . O3 . 83.6(3) yes
O5 4_656 Na1 . O5 . 168.3(2) yes
O11 3_655 Na1 . O5 . 95.6(3) yes
O11 2_546 Na1 . O5 . 87.0(4) yes
O3 . Na1 . O5 . 88.1(3) yes
O5 4_656 Na1 . O6 . 89.4(2) yes
O11 3_655 Na1 . O6 . 88.5(2) yes
O11 2_546 Na1 . O6 . 81.7(2) yes
O3 . Na1 . O6 . 161.5(5) yes
O5 . Na1 . O6 . 79.9(3) yes
O12 3_655 Na2 . O31 . 76.7(3) yes
O12 3_655 Na2 . O41 . 90.4(3) yes
O31 . Na2 . O41 . 70.2(2) yes
O12 3_655 Na2 . O2 . 85.8(3) yes
O31 . Na2 . O2 . 87.2(2) yes
O41 . Na2 . O2 . 157.35(19) yes
O12 3_655 Na2 . O3 . 84.5(3) yes
O31 . Na2 . O3 . 161.2(4) yes
O41 . Na2 . O3 . 110.8(2) yes
O2 . Na2 . O3 . 91.1(2) yes
O12 3_655 Na2 . O4 . 172.43(18) yes
O31 . Na2 . O4 . 97.6(3) yes
O41 . Na2 . O4 . 92.3(3) yes
O2 . Na2 . O4 . 89.0(4) yes
O3 . Na2 . O4 . 101.1(3) yes
O4 3_656 Na3 . O6 4_646 83.3(3) yes
O4 3_656 Na3 . O6 2_445 87.2(3) yes
O6 4_646 Na3 . O6 2_445 164.8(7) yes
O4 3_656 Na3 . O41 1_545 162.2(3) yes
O6 4_646 Na3 . O41 1_545 111.0(3) yes
O6 2_445 Na3 . O41 1_545 80.8(3) yes
O4 3_656 Na3 . O41 3_646 89.2(3) yes
O6 4_646 Na3 . O41 3_646 80.8(3) yes
O6 2_445 Na3 . O41 3_646 111.0(3) yes
O41 1_545 Na3 . O41 3_646 83.0(4) yes
O4 3_656 Na3 . O4 . 102.4(6) yes
O6 4_646 Na3 . O4 . 87.2(3) yes
O6 2_445 Na3 . O4 . 83.3(3) yes
O41 1_545 Na3 . O4 . 89.2(3) yes
O41 3_646 Na3 . O4 . 162.2(3) yes
O11 . C1 . O12 . 125.1(6) yes
O11 . C1 . C2 . 119.8(4) yes
O12 . C1 . C2 . 115.1(4) yes
Na1 3_655 O11 . Na1 2_454 88.79(11) yes
Na1 3_655 O11 . C1 . 120.2(9) yes
Na1 2_454 O11 . C1 . 117.5(10) yes
Mn1 . O12 . C1 . 102.1(3) yes
Mn1 . O12 . Na2 3_655 83.1(3) yes
C1 . O12 . Na2 3_655 131.6(10) yes
C1 . C2 . O21 . 109.4(5) yes
C1 . C2 . C3 . 107.8(11) yes
O21 . C2 . C3 . 105.6(6) yes
C1 . C2 . H2 . 111.3 no
O21 . C2 . H2 . 110.9 no
C3 . C2 . H2 . 111.6 no
C2 . O21 . Mn1 . 102.5(8) yes
C2 . C3 . O31 . 106.9(6) yes
C2 . C3 . C4 . 110.5(10) yes
O31 . C3 . C4 . 112.2(5) yes
C2 . C3 . H3 . 109.2 no
O31 . C3 . H3 . 108.7 no
C4 . C3 . H3 . 109.4 no
Na2 . O31 . C3 . 117.1(3) yes
Na2 . O31 . Mn1 . 102.7(2) yes
C3 . O31 . Mn1 . 110.0(8) yes
C3 . C4 . O41 . 119.7(7) yes
C3 . C4 . O42 . 115.6(5) yes
O41 . C4 . O42 . 124.7(5) yes
Na2 . O41 . Na3 1_565 108.8(2) yes
Na2 . O41 . C4 . 118.4(5) yes
Na3 1_565 O41 . C4 . 114.7(10) yes
H11 . O1 . H12 . 92.8 no
Na2 . O2 . H21 . 140.1 no
Na2 . O2 . H22 . 91.3 no
H21 . O2 . H22 . 105.8 no
Na2 . O3 . Na1 . 115.4(3) yes
Na2 . O3 . H31 . 95.7 no
Na1 . O3 . H31 . 103.9 no
Na2 . O3 . H32 . 92.9 no
Na1 . O3 . H32 . 120.8 no
H31 . O3 . H32 . 124.8 no
Na2 . O4 . Na3 . 121.9(2) yes
Na2 . O4 . H41 . 107.9 no
Na3 . O4 . H41 . 110.0 no
Na2 . O4 . H42 . 108.2 no
Na3 . O4 . H42 . 116.9 no
H41 . O4 . H42 . 85.8 no
Na1 4_646 O5 . Na1 . 95.46(12) yes
Na1 4_646 O5 . H51 . 120.6 no
Na1 . O5 . H51 . 102.2 no
Na1 4_646 O5 . H52 . 105.5 no
Na1 . O5 . H52 . 106.2 no
H51 . O5 . H52 . 122.2 no
Na3 2_555 O6 . Na1 . 175.5(5) yes
Na3 2_555 O6 . H61 . 85.3 no
Na1 . O6 . H61 . 94.2 no
Na3 2_555 O6 . H62 . 90.4 no
Na1 . O6 . H62 . 85.9 no
H61 . O6 . H62 . 119.1 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-6 0 4 x .
-5 -3 10 x .
-13 -3 9 x .
-3 -3 10 x .
-15 -3 9 x .
-17 -3 7 x .
-9 3 9 x .
3 -3 9 x .
-5 -3 11 x .
-17 -3 8 x .
3 3 8 x .
-11 3 9 x .
-8 0 4 x .
-17 3 8 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1419431'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_3                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_3                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_3                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_3                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_3                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_3                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_3                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

#end of refcif 
_cell_length_a                   20.0669(14)
_cell_length_b                   6.771(2)
_cell_length_c                   9.5645(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.161(4)
_cell_angle_gamma                90
_cell_volume                     1194.9(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.88 Fooo =    696.00 Mu =      7.51 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.88 FOOO =    696.00 Mu =      7.51 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.751

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4715
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         800
_diffrn_reflns_number            4120
_reflns_number_total             1029
_diffrn_reflns_av_R_equivalents  0.046
# Number of reflections without Friedels Law is 1029 
# Number of reflections with Friedels Law is 639 
# Theoretical number of reflections is about 1225 


_diffrn_reflns_theta_min         1.583
_diffrn_reflns_theta_max         17.692
_diffrn_measured_fraction_theta_max 0.478

_diffrn_reflns_theta_full        14.154
_diffrn_measured_fraction_theta_full 0.493


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.52
_refine_diff_density_max         0.43


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         1019
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0499
_refine_ls_wR_factor_ref         0.0609
_refine_ls_goodness_of_fit_ref   0.9857
_refine_ls_shift/su_max          0.0004161
_refine_ls_shift/su_mean         0.0000413


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1019
_refine_ls_R_factor_all          0.0499
_refine_ls_wR_factor_all         0.0609

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                924
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_gt          0.0597

_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_abs_structure_details 'Flack (1983), 390 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8046(4) 0.0000 0.0258 1.0000 Uani S T . . . .
Na1 Na 0.73765(7) 0.5500(9) 0.49171(17) 0.0275 1.0000 Uani . . . . . .
Na2 Na 0.52320(6) 0.4923(7) 0.28360(14) 0.0293 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0239(10) 0.5000 0.0379 1.0000 Uani S T . . . .
C1 C 0.35262(14) 0.8337(19) -0.2098(3) 0.0227 1.0000 Uani . U . . . .
O11 O 0.28897(10) 0.8026(15) -0.3020(2) 0.0337 1.0000 Uani . U . . . .
O12 O 0.40841(10) 0.8094(15) -0.2405(2) 0.0246 1.0000 Uani . U . . . .
C2 C 0.36724(15) 0.8938(16) -0.0447(4) 0.0228 1.0000 Uani . U . . . .
O21 O 0.43402(11) 0.9903(13) 0.0200(2) 0.0253 1.0000 Uani . U . . . .
C3 C 0.37737(15) 0.7019(17) 0.0456(4) 0.0240 1.0000 Uani . U . . . .
O31 O 0.44246(11) 0.6093(12) 0.0489(2) 0.0248 1.0000 Uani . U . . . .
C4 C 0.38064(16) 0.749(2) 0.2070(4) 0.0232 1.0000 Uani . U . . . .
O41 O 0.43474(13) 0.6946(12) 0.3203(3) 0.0279 1.0000 Uani . U . . . .
O42 O 0.32535(13) 0.8261(16) 0.2105(3) 0.0484 1.0000 Uani . U . . . .
O1 O 0.81006(13) 0.7801(17) 0.1570(3) 0.0653 1.0000 Uani . . . . . .
O2 O 0.58050(10) 0.3217(14) 0.1463(2) 0.0285 1.0000 Uani . U . . . .
O3 O 0.62493(13) 0.4536(13) 0.5075(3) 0.0296 1.0000 Uani . U . . . .
O4 O 0.45891(12) 0.1944(12) 0.2882(3) 0.0304 1.0000 Uani . U . . . .
O5 O 0.72128(10) 0.2904(15) 0.3234(2) 0.0329 1.0000 Uani . U . . . .
O6 O 0.87258(14) 0.5277(14) 0.4915(3) 0.0277 1.0000 Uani . U . . . .
H2 H 0.3270 0.9759 -0.0389 0.0270 1.0000 Uiso . . . . . .
H3 H 0.3352 0.6132 -0.0075 0.0285 1.0000 Uiso . . . . . .
H11 H 0.7808 0.7867 0.1999 0.0983 1.0000 Uiso . . . . . .
H12 H 0.8142 0.6575 0.1715 0.0983 1.0000 Uiso . . . . . .
H21 H 0.5760 0.2185 0.0945 0.0425 1.0000 Uiso . . . . . .
H22 H 0.5731 0.4142 0.0834 0.0425 1.0000 Uiso . . . . . .
H31 H 0.6257 0.3289 0.5079 0.0448 1.0000 Uiso . . . . . .
H32 H 0.6076 0.5232 0.5575 0.0448 1.0000 Uiso . . . . . .
H41 H 0.4514 0.1328 0.2071 0.0456 1.0000 Uiso . . . . . .
H42 H 0.4143 0.2201 0.2489 0.0456 1.0000 Uiso . . . . . .
H51 H 0.6770 0.3003 0.2677 0.0495 1.0000 Uiso . . . . . .
H52 H 0.7535 0.3016 0.2884 0.0495 1.0000 Uiso . . . . . .
H61 H 0.8585 0.4680 0.4079 0.0417 1.0000 Uiso . . . . . .
H62 H 0.8833 0.4623 0.5719 0.0417 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2864(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.3119(19) yes
Mn1 . O31 3_655 1.930(6) yes
Mn1 . O21 3_655 1.889(7) yes
Mn1 . O12 . 2.3119(19) yes
Mn1 . O21 . 1.889(7) yes
Mn1 . O31 . 1.930(6) yes
Na1 . O5 4_656 2.304(9) yes
Na1 . O11 3_655 2.396(9) yes
Na1 . O11 2_546 2.482(8) yes
Na1 . O3 . 2.415(4) yes
Na1 . O5 . 2.318(9) yes
Na1 . O6 . 2.713(3) yes
Na2 . O12 3_655 2.666(9) yes
Na2 . O31 . 2.330(4) yes
Na2 . O41 . 2.375(6) yes
Na2 . O2 . 2.360(6) yes
Na2 . O3 . 2.320(3) yes
Na2 . O4 . 2.404(8) yes
Na3 . O4 3_656 2.379(7) yes
Na3 . O6 4_646 2.550(3) yes
Na3 . O6 2_445 2.550(3) yes
Na3 . O41 1_545 2.555(8) yes
Na3 . O41 3_646 2.555(8) yes
Na3 . O4 . 2.379(7) yes
C1 . O11 . 1.252(4) yes
C1 . O12 . 1.275(4) yes
C1 . C2 . 1.543(6) yes
C2 . O21 . 1.397(8) yes
C2 . C3 . 1.529(15) yes
C2 . H2 . 1.000 no
C3 . O31 . 1.438(7) yes
C3 . C4 . 1.552(6) yes
C3 . H3 . 0.998 no
C4 . O41 . 1.250(6) yes
C4 . O42 . 1.239(7) yes
O1 . H11 . 0.840 no
O1 . H12 . 0.840 no
O2 . H21 . 0.841 no
O2 . H22 . 0.840 no
O3 . H31 . 0.844 no
O3 . H32 . 0.838 no
O4 . H41 . 0.840 no
O4 . H42 . 0.841 no
O5 . H51 . 0.840 no
O5 . H52 . 0.840 no
O6 . H61 . 0.839 no
O6 . H62 . 0.839 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.18(19) yes
O12 3_655 Mn1 . O21 3_655 77.1(2) yes
O31 3_655 Mn1 . O21 3_655 85.5(2) yes
O12 3_655 Mn1 . O12 . 178.4(5) yes
O31 3_655 Mn1 . O12 . 94.9(2) yes
O21 3_655 Mn1 . O12 . 101.8(2) yes
O12 3_655 Mn1 . O21 . 101.8(2) yes
O31 3_655 Mn1 . O21 . 172.01(12) yes
O21 3_655 Mn1 . O21 . 96.6(4) yes
O12 . Mn1 . O21 . 77.1(2) yes
O12 3_655 Mn1 . O31 . 94.9(2) yes
O31 3_655 Mn1 . O31 . 93.5(4) yes
O21 3_655 Mn1 . O31 . 172.01(12) yes
O12 . Mn1 . O31 . 86.18(19) yes
O21 . Mn1 . O31 . 85.5(2) yes
O5 4_656 Na1 . O11 3_655 89.0(4) yes
O5 4_656 Na1 . O11 2_546 87.5(2) yes
O11 3_655 Na1 . O11 2_546 169.41(14) yes
O5 4_656 Na1 . O3 . 101.78(18) yes
O11 3_655 Na1 . O3 . 107.76(18) yes
O11 2_546 Na1 . O3 . 82.75(19) yes
O5 4_656 Na1 . O5 . 168.20(16) yes
O11 3_655 Na1 . O5 . 94.98(19) yes
O11 2_546 Na1 . O5 . 86.6(3) yes
O3 . Na1 . O5 . 87.6(2) yes
O5 4_656 Na1 . O6 . 89.09(18) yes
O11 3_655 Na1 . O6 . 87.96(18) yes
O11 2_546 Na1 . O6 . 82.00(18) yes
O3 . Na1 . O6 . 160.8(4) yes
O5 . Na1 . O6 . 79.99(19) yes
O12 3_655 Na2 . O31 . 77.4(2) yes
O12 3_655 Na2 . O41 . 91.1(2) yes
O31 . Na2 . O41 . 70.71(16) yes
O12 3_655 Na2 . O2 . 85.1(3) yes
O31 . Na2 . O2 . 86.36(17) yes
O41 . Na2 . O2 . 157.03(13) yes
O12 3_655 Na2 . O3 . 85.1(2) yes
O31 . Na2 . O3 . 162.5(3) yes
O41 . Na2 . O3 . 111.49(18) yes
O2 . Na2 . O3 . 90.79(15) yes
O12 3_655 Na2 . O4 . 172.33(13) yes
O31 . Na2 . O4 . 97.3(2) yes
O41 . Na2 . O4 . 92.50(19) yes
O2 . Na2 . O4 . 89.0(3) yes
O3 . Na2 . O4 . 99.9(3) yes
O4 3_656 Na3 . O6 4_646 83.12(18) yes
O4 3_656 Na3 . O6 2_445 87.09(19) yes
O6 4_646 Na3 . O6 2_445 164.2(5) yes
O4 3_656 Na3 . O41 1_545 161.95(19) yes
O6 4_646 Na3 . O41 1_545 111.5(2) yes
O6 2_445 Na3 . O41 1_545 80.7(2) yes
O4 3_656 Na3 . O41 3_646 88.65(18) yes
O6 4_646 Na3 . O41 3_646 80.7(2) yes
O6 2_445 Na3 . O41 3_646 111.5(2) yes
O41 1_545 Na3 . O41 3_646 83.5(3) yes
O4 3_656 Na3 . O4 . 103.1(4) yes
O6 4_646 Na3 . O4 . 87.09(19) yes
O6 2_445 Na3 . O4 . 83.12(18) yes
O41 1_545 Na3 . O4 . 88.65(18) yes
O41 3_646 Na3 . O4 . 161.95(19) yes
O11 . C1 . O12 . 124.1(4) yes
O11 . C1 . C2 . 119.8(3) yes
O12 . C1 . C2 . 116.1(3) yes
Na1 3_655 O11 . Na1 2_454 88.90(7) yes
Na1 3_655 O11 . C1 . 121.0(6) yes
Na1 2_454 O11 . C1 . 115.8(7) yes
Mn1 . O12 . C1 . 101.47(18) yes
Mn1 . O12 . Na2 3_655 83.5(2) yes
C1 . O12 . Na2 3_655 133.8(7) yes
C1 . C2 . O21 . 109.9(3) yes
C1 . C2 . C3 . 106.5(8) yes
O21 . C2 . C3 . 104.8(4) yes
C1 . C2 . H2 . 111.7 no
O21 . C2 . H2 . 111.8 no
C3 . C2 . H2 . 111.8 no
C2 . O21 . Mn1 . 103.4(6) yes
C2 . C3 . O31 . 107.5(4) yes
C2 . C3 . C4 . 109.4(9) yes
O31 . C3 . C4 . 112.7(3) yes
C2 . C3 . H3 . 109.0 no
O31 . C3 . H3 . 109.2 no
C4 . C3 . H3 . 109.0 no
Na2 . O31 . C3 . 116.8(2) yes
Na2 . O31 . Mn1 . 102.16(14) yes
C3 . O31 . Mn1 . 108.7(6) yes
C3 . C4 . O41 . 119.0(6) yes
C3 . C4 . O42 . 115.1(4) yes
O41 . C4 . O42 . 125.6(4) yes
Na2 . O41 . Na3 1_565 108.32(13) yes
Na2 . O41 . C4 . 119.1(4) yes
Na3 1_565 O41 . C4 . 113.9(8) yes
H11 . O1 . H12 . 90.8 no
Na2 . O2 . H21 . 140.5 no
Na2 . O2 . H22 . 92.7 no
H21 . O2 . H22 . 104.5 no
Na2 . O3 . Na1 . 114.67(18) yes
Na2 . O3 . H31 . 97.2 no
Na1 . O3 . H31 . 104.8 no
Na2 . O3 . H32 . 93.0 no
Na1 . O3 . H32 . 119.5 no
H31 . O3 . H32 . 124.8 no
Na3 . O4 . Na2 . 121.90(16) yes
Na3 . O4 . H41 . 110.7 no
Na2 . O4 . H41 . 107.7 no
Na3 . O4 . H42 . 117.4 no
Na2 . O4 . H42 . 107.6 no
H41 . O4 . H42 . 85.2 no
Na1 4_646 O5 . Na1 . 95.31(8) yes
Na1 4_646 O5 . H51 . 120.8 no
Na1 . O5 . H51 . 101.9 no
Na1 4_646 O5 . H52 . 105.7 no
Na1 . O5 . H52 . 106.7 no
H51 . O5 . H52 . 121.9 no
Na3 2_555 O6 . Na1 . 175.0(4) yes
Na3 2_555 O6 . H61 . 85.5 no
Na1 . O6 . H61 . 93.8 no
Na3 2_555 O6 . H62 . 90.3 no
Na1 . O6 . H62 . 85.7 no
H61 . O6 . H62 . 119.2 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1419432'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_4                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_4                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_4                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_4                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_4                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_4                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_4                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

#end of refcif 
_cell_length_a                   20.0069(12)
_cell_length_b                   6.7361(19)
_cell_length_c                   9.5511(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.257(4)
_cell_angle_gamma                90
_cell_volume                     1182.6(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.90 Fooo =    696.00 Mu =      7.59 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.90 FOOO =    696.00 Mu =      7.59 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.759

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4657
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1090
_diffrn_reflns_number            4041
_reflns_number_total             1052
_diffrn_reflns_av_R_equivalents  0.051
# Number of reflections without Friedels Law is 1052 
# Number of reflections with Friedels Law is 649 
# Theoretical number of reflections is about 1211 


_diffrn_reflns_theta_min         1.587
_diffrn_reflns_theta_max         17.686
_diffrn_measured_fraction_theta_max 0.490

_diffrn_reflns_theta_full        14.326
_diffrn_measured_fraction_theta_full 0.501


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.30


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         1025
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0582
_refine_ls_wR_factor_ref         0.0719
_refine_ls_goodness_of_fit_ref   0.9863
_refine_ls_shift/su_max          0.0004883
_refine_ls_shift/su_mean         0.0000466


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1025
_refine_ls_R_factor_all          0.0582
_refine_ls_wR_factor_all         0.0719

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                914
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_gt          0.0710

_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_abs_structure_details 'Flack (1983), 403 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8053(5) 0.0000 0.0288 1.0000 Uani S T . . . .
Na1 Na 0.73752(9) 0.5501(10) 0.4919(2) 0.0318 1.0000 Uani . . . . . .
Na2 Na 0.52297(8) 0.4934(9) 0.28434(16) 0.0307 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0222(11) 0.5000 0.0383 1.0000 Uani S T . . . .
C1 C 0.35230(17) 0.834(2) -0.2097(4) 0.0303 1.0000 Uani . U . . . .
O11 O 0.28838(12) 0.8016(18) -0.3027(3) 0.0385 1.0000 Uani . U . . . .
O12 O 0.40848(12) 0.8121(18) -0.2412(3) 0.0291 1.0000 Uani . U . . . .
C2 C 0.36690(18) 0.892(2) -0.0453(4) 0.0275 1.0000 Uani . U . . . .
O21 O 0.43401(13) 0.9905(15) 0.0204(3) 0.0294 1.0000 Uani . U . . . .
C3 C 0.37693(18) 0.698(2) 0.0443(4) 0.0285 1.0000 Uani . U . . . .
O31 O 0.44226(13) 0.6076(15) 0.0491(3) 0.0290 1.0000 Uani . U . . . .
C4 C 0.3797(2) 0.749(2) 0.2061(4) 0.0294 1.0000 Uani . U . . . .
O41 O 0.43421(15) 0.6960(14) 0.3205(3) 0.0327 1.0000 Uani . U . . . .
O42 O 0.32414(15) 0.8248(19) 0.2084(3) 0.0511 1.0000 Uani . U . . . .
O1 O 0.80996(15) 0.780(2) 0.1556(4) 0.0673 1.0000 Uani . . . . . .
O2 O 0.57999(12) 0.3213(16) 0.1469(3) 0.0330 1.0000 Uani . U . . . .
O3 O 0.62460(15) 0.4539(15) 0.5081(3) 0.0349 1.0000 Uani . U . . . .
O4 O 0.45866(14) 0.1964(15) 0.2882(3) 0.0355 1.0000 Uani . U . . . .
O5 O 0.72092(12) 0.2876(17) 0.3229(3) 0.0379 1.0000 Uani . U . . . .
O6 O 0.87208(16) 0.5270(16) 0.4909(3) 0.0318 1.0000 Uani . U . . . .
H2 H 0.3262 0.9717 -0.0393 0.0364 1.0000 Uiso . . . . . .
H3 H 0.3353 0.6054 -0.0091 0.0375 1.0000 Uiso . . . . . .
H11 H 0.7810 0.7895 0.2000 0.1026 1.0000 Uiso . . . . . .
H12 H 0.8140 0.6607 0.1707 0.1026 1.0000 Uiso . . . . . .
H21 H 0.5755 0.2172 0.0949 0.0510 1.0000 Uiso . . . . . .
H22 H 0.5728 0.4126 0.0842 0.0510 1.0000 Uiso . . . . . .
H31 H 0.6255 0.3299 0.5073 0.0541 1.0000 Uiso . . . . . .
H32 H 0.6072 0.5248 0.5572 0.0541 1.0000 Uiso . . . . . .
H41 H 0.4512 0.1334 0.2068 0.0551 1.0000 Uiso . . . . . .
H42 H 0.4140 0.2221 0.2484 0.0551 1.0000 Uiso . . . . . .
H51 H 0.6765 0.2971 0.2676 0.0578 1.0000 Uiso . . . . . .
H52 H 0.7530 0.2984 0.2874 0.0578 1.0000 Uiso . . . . . .
H61 H 0.8577 0.4667 0.4072 0.0492 1.0000 Uiso . . . . . .
H62 H 0.8830 0.4620 0.5723 0.0492 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2788(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.309(2) yes
Mn1 . O31 3_655 1.938(8) yes
Mn1 . O21 3_655 1.881(8) yes
Mn1 . O12 . 2.309(2) yes
Mn1 . O21 . 1.881(8) yes
Mn1 . O31 . 1.938(8) yes
Na1 . O5 4_656 2.285(10) yes
Na1 . O11 3_655 2.381(11) yes
Na1 . O11 2_546 2.471(10) yes
Na1 . O3 . 2.413(4) yes
Na1 . O5 . 2.328(11) yes
Na1 . O6 . 2.701(4) yes
Na2 . O12 3_655 2.666(11) yes
Na2 . O31 . 2.320(5) yes
Na2 . O41 . 2.371(6) yes
Na2 . O2 . 2.356(7) yes
Na2 . O3 . 2.311(3) yes
Na2 . O4 . 2.387(9) yes
Na3 . O4 3_656 2.372(8) yes
Na3 . O6 4_646 2.548(3) yes
Na3 . O6 2_445 2.548(3) yes
Na3 . O41 1_545 2.548(10) yes
Na3 . O41 3_646 2.548(10) yes
Na3 . O4 . 2.372(8) yes
C1 . O11 . 1.255(5) yes
C1 . O12 . 1.282(5) yes
C1 . C2 . 1.530(7) yes
C2 . O21 . 1.404(9) yes
C2 . C3 . 1.532(18) yes
C2 . H2 . 0.995 no
C3 . O31 . 1.426(8) yes
C3 . C4 . 1.563(7) yes
C3 . H3 . 1.003 no
C4 . O41 . 1.253(7) yes
C4 . O42 . 1.231(8) yes
O1 . H11 . 0.845 no
O1 . H12 . 0.813 no
O2 . H21 . 0.843 no
O2 . H22 . 0.830 no
O3 . H31 . 0.835 no
O3 . H32 . 0.835 no
O4 . H41 . 0.846 no
O4 . H42 . 0.839 no
O5 . H51 . 0.838 no
O5 . H52 . 0.839 no
O6 . H61 . 0.840 no
O6 . H62 . 0.843 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.7(2) yes
O12 3_655 Mn1 . O21 3_655 77.1(2) yes
O31 3_655 Mn1 . O21 3_655 85.5(2) yes
O12 3_655 Mn1 . O12 . 177.7(6) yes
O31 3_655 Mn1 . O12 . 94.9(2) yes
O21 3_655 Mn1 . O12 . 101.3(2) yes
O12 3_655 Mn1 . O21 . 101.3(2) yes
O31 3_655 Mn1 . O21 . 172.01(15) yes
O21 3_655 Mn1 . O21 . 97.0(5) yes
O12 . Mn1 . O21 . 77.1(2) yes
O12 3_655 Mn1 . O31 . 94.9(2) yes
O31 3_655 Mn1 . O31 . 93.2(5) yes
O21 3_655 Mn1 . O31 . 172.01(15) yes
O12 . Mn1 . O31 . 86.7(2) yes
O21 . Mn1 . O31 . 85.5(2) yes
O5 4_656 Na1 . O11 3_655 89.6(4) yes
O5 4_656 Na1 . O11 2_546 87.1(2) yes
O11 3_655 Na1 . O11 2_546 169.30(15) yes
O5 4_656 Na1 . O3 . 101.7(2) yes
O11 3_655 Na1 . O3 . 108.1(2) yes
O11 2_546 Na1 . O3 . 82.5(2) yes
O5 4_656 Na1 . O5 . 167.8(2) yes
O11 3_655 Na1 . O5 . 94.9(2) yes
O11 2_546 Na1 . O5 . 86.4(4) yes
O3 . Na1 . O5 . 87.7(3) yes
O5 4_656 Na1 . O6 . 89.1(2) yes
O11 3_655 Na1 . O6 . 87.5(2) yes
O11 2_546 Na1 . O6 . 82.3(2) yes
O3 . Na1 . O6 . 160.8(5) yes
O5 . Na1 . O6 . 79.8(2) yes
O12 3_655 Na2 . O31 . 77.7(2) yes
O12 3_655 Na2 . O41 . 91.1(3) yes
O31 . Na2 . O41 . 71.04(19) yes
O12 3_655 Na2 . O2 . 85.3(3) yes
O31 . Na2 . O2 . 85.9(2) yes
O41 . Na2 . O2 . 156.91(15) yes
O12 3_655 Na2 . O3 . 85.2(3) yes
O31 . Na2 . O3 . 162.9(4) yes
O41 . Na2 . O3 . 111.6(2) yes
O2 . Na2 . O3 . 90.89(18) yes
O12 3_655 Na2 . O4 . 172.24(15) yes
O31 . Na2 . O4 . 96.9(2) yes
O41 . Na2 . O4 . 92.3(2) yes
O2 . Na2 . O4 . 88.8(3) yes
O3 . Na2 . O4 . 99.9(3) yes
O4 3_656 Na3 . O6 4_646 83.3(2) yes
O4 3_656 Na3 . O6 2_445 87.5(2) yes
O6 4_646 Na3 . O6 2_445 165.0(6) yes
O4 3_656 Na3 . O41 1_545 161.8(2) yes
O6 4_646 Na3 . O41 1_545 111.4(3) yes
O6 2_445 Na3 . O41 1_545 80.2(2) yes
O4 3_656 Na3 . O41 3_646 88.6(2) yes
O6 4_646 Na3 . O41 3_646 80.2(2) yes
O6 2_445 Na3 . O41 3_646 111.4(3) yes
O41 1_545 Na3 . O41 3_646 83.7(4) yes
O4 3_656 Na3 . O4 . 103.2(5) yes
O6 4_646 Na3 . O4 . 87.5(2) yes
O6 2_445 Na3 . O4 . 83.3(2) yes
O41 1_545 Na3 . O4 . 88.6(2) yes
O41 3_646 Na3 . O4 . 161.8(2) yes
O11 . C1 . O12 . 123.9(5) yes
O11 . C1 . C2 . 119.9(3) yes
O12 . C1 . C2 . 116.1(3) yes
Na1 3_655 O11 . Na1 2_454 88.92(8) yes
Na1 3_655 O11 . C1 . 121.0(7) yes
Na1 2_454 O11 . C1 . 115.5(9) yes
Mn1 . O12 . C1 . 101.0(2) yes
Mn1 . O12 . Na2 3_655 83.4(2) yes
C1 . O12 . Na2 3_655 132.8(9) yes
C1 . C2 . O21 . 109.9(4) yes
C1 . C2 . C3 . 106.5(10) yes
O21 . C2 . C3 . 105.2(5) yes
C1 . C2 . H2 . 111.6 no
O21 . C2 . H2 . 112.2 no
C3 . C2 . H2 . 111.0 no
C2 . O21 . Mn1 . 103.1(7) yes
C2 . C3 . O31 . 107.3(5) yes
C2 . C3 . C4 . 108.0(10) yes
O31 . C3 . C4 . 112.8(4) yes
C2 . C3 . H3 . 110.3 no
O31 . C3 . H3 . 108.6 no
C4 . C3 . H3 . 109.7 no
Na2 . O31 . C3 . 116.8(2) yes
Na2 . O31 . Mn1 . 102.05(17) yes
C3 . O31 . Mn1 . 109.0(8) yes
C3 . C4 . O41 . 118.5(7) yes
C3 . C4 . O42 . 115.4(4) yes
O41 . C4 . O42 . 125.7(4) yes
Na2 . O41 . Na3 1_565 108.01(15) yes
Na2 . O41 . C4 . 118.8(5) yes
Na3 1_565 O41 . C4 . 114.5(9) yes
H11 . O1 . H12 . 91.6 no
Na2 . O2 . H21 . 140.8 no
Na2 . O2 . H22 . 93.0 no
H21 . O2 . H22 . 104.1 no
Na2 . O3 . Na1 . 114.5(2) yes
Na2 . O3 . H31 . 97.0 no
Na1 . O3 . H31 . 104.1 no
Na2 . O3 . H32 . 92.5 no
Na1 . O3 . H32 . 119.3 no
H31 . O3 . H32 . 126.3 no
Na3 . O4 . Na2 . 121.67(19) yes
Na3 . O4 . H41 . 110.4 no
Na2 . O4 . H41 . 107.9 no
Na3 . O4 . H42 . 117.7 no
Na2 . O4 . H42 . 107.7 no
H41 . O4 . H42 . 85.3 no
Na1 . O5 . Na1 4_646 94.95(9) yes
Na1 . O5 . H51 . 101.8 no
Na1 4_646 O5 . H51 . 120.8 no
Na1 . O5 . H52 . 107.0 no
Na1 4_646 O5 . H52 . 105.7 no
H51 . O5 . H52 . 122.0 no
Na3 2_555 O6 . Na1 . 175.4(5) yes
Na3 2_555 O6 . H61 . 86.1 no
Na1 . O6 . H61 . 93.7 no
Na3 2_555 O6 . H62 . 90.6 no
Na1 . O6 . H62 . 85.5 no
H61 . O6 . H62 . 119.6 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-21 3 1 x .
-21 3 5 x .
-17 3 8 x .
17 3 2 x .
-1 -3 10 x .
-3 -3 10 x .
-5 -3 10 x .
-17 3 7 x .
13 3 5 x .
-21 3 3 x .
19 3 1 x .
2 -2 5 x .
-21 3 4 x .
-21 3 2 x .
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1419433'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_5                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_5                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_5                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_5                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_5                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_5                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_5                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.9615(16)
_cell_length_b                   6.715(3)
_cell_length_c                   9.5408(8)
_cell_angle_alpha                90
_cell_angle_beta                 113.331(4)
_cell_angle_gamma                90
_cell_volume                     1174.3(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.92 Fooo =    696.00 Mu =      7.65 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.92 FOOO =    696.00 Mu =      7.65 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.765

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4576
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1320
_diffrn_reflns_number            3903
_reflns_number_total             1026
_diffrn_reflns_av_R_equivalents  0.058
# Number of reflections without Friedels Law is 1026 
# Number of reflections with Friedels Law is 645 
# Theoretical number of reflections is about 1201 


_diffrn_reflns_theta_min         1.589
_diffrn_reflns_theta_max         17.677
_diffrn_measured_fraction_theta_max 0.492

_diffrn_reflns_theta_full        14.495
_diffrn_measured_fraction_theta_full 0.504


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.50
_refine_diff_density_max         0.41


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         1015
_refine_ls_number_restraints     131
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0587
_refine_ls_wR_factor_ref         0.0707
_refine_ls_goodness_of_fit_ref   0.9972
_refine_ls_shift/su_max          0.0003265
_refine_ls_shift/su_mean         0.0000350


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        1015
_refine_ls_R_factor_all          0.0587
_refine_ls_wR_factor_all         0.0707

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                909
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_gt          0.0696

_refine_ls_abs_structure_Flack   0.13(6)
_refine_ls_abs_structure_details 'Flack (1983), 381 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8055(5) 0.0000 0.0240 1.0000 Uani S T . . . .
Na1 Na 0.73743(8) 0.5475(10) 0.4916(2) 0.0342 1.0000 Uani . . . . . .
Na2 Na 0.52278(7) 0.4938(8) 0.28478(15) 0.0331 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0236(11) 0.5000 0.0403 1.0000 Uani S T . . . .
C1 C 0.35191(16) 0.832(2) -0.2106(3) 0.0282 1.0000 Uani . U . . . .
O11 O 0.28807(11) 0.8000(17) -0.3033(2) 0.0365 1.0000 Uani . U . . . .
O12 O 0.40851(11) 0.8088(18) -0.2415(2) 0.0327 1.0000 Uani . U . . . .
C2 C 0.36663(17) 0.8922(19) -0.0455(4) 0.0281 1.0000 Uani . U . . . .
O21 O 0.43416(12) 0.9926(15) 0.0203(3) 0.0310 1.0000 Uani . U . . . .
C3 C 0.37621(17) 0.6975(19) 0.0440(4) 0.0302 1.0000 Uani . U . . . .
O31 O 0.44202(13) 0.6088(14) 0.0487(3) 0.0300 1.0000 Uani . U . . . .
C4 C 0.37939(19) 0.747(2) 0.2062(4) 0.0331 1.0000 Uani . U . . . .
O41 O 0.43356(14) 0.6978(14) 0.3203(3) 0.0335 1.0000 Uani . U . . . .
O42 O 0.32324(14) 0.8255(18) 0.2071(3) 0.0479 1.0000 Uani . U . . . .
O1 O 0.80930(14) 0.7870(19) 0.1540(3) 0.0521 1.0000 Uani . . . . . .
O2 O 0.57954(12) 0.3211(16) 0.1475(3) 0.0292 1.0000 Uani . U . . . .
O3 O 0.62485(14) 0.4545(14) 0.5083(3) 0.0316 1.0000 Uani . U . . . .
O4 O 0.45837(13) 0.1966(14) 0.2883(3) 0.0342 1.0000 Uani . U . . . .
O5 O 0.72059(11) 0.2863(16) 0.3229(3) 0.0360 1.0000 Uani . U . . . .
O6 O 0.87178(16) 0.5278(16) 0.4902(3) 0.0326 1.0000 Uani . U . . . .
H2 H 0.3259 0.9742 -0.0403 0.0331 1.0000 Uiso . . . . . .
H3 H 0.3341 0.6074 -0.0100 0.0359 1.0000 Uiso . . . . . .
H11 H 0.7804 0.7904 0.1983 0.0775 1.0000 Uiso . . . . . .
H12 H 0.8130 0.6629 0.1682 0.0775 1.0000 Uiso . . . . . .
H21 H 0.5753 0.2181 0.0948 0.0430 1.0000 Uiso . . . . . .
H22 H 0.5726 0.4141 0.0842 0.0430 1.0000 Uiso . . . . . .
H31 H 0.6258 0.3292 0.5088 0.0482 1.0000 Uiso . . . . . .
H32 H 0.6077 0.5256 0.5586 0.0482 1.0000 Uiso . . . . . .
H41 H 0.4510 0.1348 0.2069 0.0513 1.0000 Uiso . . . . . .
H42 H 0.4136 0.2237 0.2479 0.0513 1.0000 Uiso . . . . . .
H51 H 0.6760 0.2975 0.2674 0.0540 1.0000 Uiso . . . . . .
H52 H 0.7525 0.2987 0.2868 0.0540 1.0000 Uiso . . . . . .
H61 H 0.8574 0.4682 0.4062 0.0489 1.0000 Uiso . . . . . .
H62 H 0.8828 0.4621 0.5710 0.0489 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2912(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.305(2) yes
Mn1 . O31 3_655 1.930(7) yes
Mn1 . O21 3_655 1.883(7) yes
Mn1 . O12 . 2.305(2) yes
Mn1 . O21 . 1.883(7) yes
Mn1 . O31 . 1.930(7) yes
Na1 . O5 4_656 2.287(9) yes
Na1 . O11 3_655 2.375(10) yes
Na1 . O11 2_546 2.458(9) yes
Na1 . O3 . 2.398(4) yes
Na1 . O5 . 2.314(10) yes
Na1 . O6 . 2.690(3) yes
Na2 . O12 3_655 2.641(10) yes
Na2 . O31 . 2.322(5) yes
Na2 . O41 . 2.375(6) yes
Na2 . O2 . 2.350(6) yes
Na2 . O3 . 2.308(3) yes
Na2 . O4 . 2.381(9) yes
Na3 . O4 3_656 2.372(8) yes
Na3 . O41 1_545 2.529(9) yes
Na3 . O41 3_646 2.529(9) yes
Na3 . O6 2_445 2.547(3) yes
Na3 . O6 4_646 2.547(3) yes
Na3 . O4 . 2.372(8) yes
C1 . O11 . 1.249(5) yes
C1 . O12 . 1.286(4) yes
C1 . C2 . 1.537(7) yes
C2 . O21 . 1.413(9) yes
C2 . C3 . 1.532(17) yes
C2 . H2 . 1.000 no
C3 . O31 . 1.427(8) yes
C3 . C4 . 1.560(7) yes
C3 . H3 . 0.998 no
C4 . O41 . 1.238(6) yes
C4 . O42 . 1.240(8) yes
O1 . H11 . 0.840 no
O1 . H12 . 0.843 no
O2 . H21 . 0.839 no
O2 . H22 . 0.841 no
O3 . H31 . 0.842 no
O3 . H32 . 0.840 no
O4 . H41 . 0.840 no
O4 . H42 . 0.842 no
O5 . H51 . 0.840 no
O5 . H52 . 0.840 no
O6 . H61 . 0.838 no
O6 . H62 . 0.838 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.2(2) yes
O12 3_655 Mn1 . O21 3_655 77.7(2) yes
O31 3_655 Mn1 . O21 3_655 85.5(2) yes
O12 3_655 Mn1 . O12 . 178.9(6) yes
O31 3_655 Mn1 . O12 . 94.5(2) yes
O21 3_655 Mn1 . O12 . 101.5(2) yes
O12 3_655 Mn1 . O21 . 101.5(2) yes
O31 3_655 Mn1 . O21 . 172.24(13) yes
O21 3_655 Mn1 . O21 . 96.3(5) yes
O12 . Mn1 . O21 . 77.7(2) yes
O12 3_655 Mn1 . O31 . 94.5(2) yes
O31 3_655 Mn1 . O31 . 93.6(5) yes
O21 3_655 Mn1 . O31 . 172.24(13) yes
O12 . Mn1 . O31 . 86.2(2) yes
O21 . Mn1 . O31 . 85.5(2) yes
O5 4_656 Na1 . O11 3_655 89.3(4) yes
O5 4_656 Na1 . O11 2_546 87.1(2) yes
O11 3_655 Na1 . O11 2_546 169.17(15) yes
O5 4_656 Na1 . O3 . 101.4(2) yes
O11 3_655 Na1 . O3 . 108.1(2) yes
O11 2_546 Na1 . O3 . 82.6(2) yes
O5 4_656 Na1 . O5 . 167.89(18) yes
O11 3_655 Na1 . O5 . 94.9(2) yes
O11 2_546 Na1 . O5 . 86.7(4) yes
O3 . Na1 . O5 . 88.1(2) yes
O5 4_656 Na1 . O6 . 88.7(2) yes
O11 3_655 Na1 . O6 . 86.9(2) yes
O11 2_546 Na1 . O6 . 82.8(2) yes
O3 . Na1 . O6 . 161.8(5) yes
O5 . Na1 . O6 . 80.2(2) yes
O12 3_655 Na2 . O31 . 77.6(2) yes
O12 3_655 Na2 . O41 . 91.4(3) yes
O31 . Na2 . O41 . 71.01(18) yes
O12 3_655 Na2 . O2 . 85.0(3) yes
O31 . Na2 . O2 . 85.8(2) yes
O41 . Na2 . O2 . 156.71(14) yes
O12 3_655 Na2 . O3 . 85.0(2) yes
O31 . Na2 . O3 . 162.5(3) yes
O41 . Na2 . O3 . 111.8(2) yes
O2 . Na2 . O3 . 90.84(17) yes
O12 3_655 Na2 . O4 . 171.96(15) yes
O31 . Na2 . O4 . 97.0(2) yes
O41 . Na2 . O4 . 92.4(2) yes
O2 . Na2 . O4 . 88.7(3) yes
O3 . Na2 . O4 . 100.1(3) yes
O4 3_656 Na3 . O41 1_545 162.0(2) yes
O4 3_656 Na3 . O41 3_646 88.3(2) yes
O41 1_545 Na3 . O41 3_646 84.6(4) yes
O4 3_656 Na3 . O6 2_445 87.4(2) yes
O41 1_545 Na3 . O6 2_445 80.0(2) yes
O41 3_646 Na3 . O6 2_445 112.0(2) yes
O4 3_656 Na3 . O6 4_646 82.9(2) yes
O41 1_545 Na3 . O6 4_646 112.0(2) yes
O41 3_646 Na3 . O6 4_646 80.0(2) yes
O6 2_445 Na3 . O6 4_646 164.4(6) yes
O4 3_656 Na3 . O4 . 102.9(5) yes
O41 1_545 Na3 . O4 . 88.3(2) yes
O41 3_646 Na3 . O4 . 162.0(2) yes
O6 2_445 Na3 . O4 . 82.9(2) yes
O6 4_646 Na3 . O4 . 87.4(2) yes
O11 . C1 . O12 . 124.0(5) yes
O11 . C1 . C2 . 119.9(3) yes
O12 . C1 . C2 . 116.0(3) yes
Na1 3_655 O11 . Na1 2_454 89.04(8) yes
Na1 3_655 O11 . C1 . 120.8(7) yes
Na1 2_454 O11 . C1 . 115.4(9) yes
Mn1 . O12 . C1 . 101.06(19) yes
Mn1 . O12 . Na2 3_655 83.9(2) yes
C1 . O12 . Na2 3_655 133.8(8) yes
C1 . C2 . O21 . 110.0(4) yes
C1 . C2 . C3 . 106.2(10) yes
O21 . C2 . C3 . 105.9(5) yes
C1 . C2 . H2 . 111.5 no
O21 . C2 . H2 . 111.5 no
C3 . C2 . H2 . 111.5 no
C2 . O21 . Mn1 . 102.6(7) yes
C2 . C3 . O31 . 106.5(5) yes
C2 . C3 . C4 . 108.5(10) yes
O31 . C3 . C4 . 112.5(4) yes
C2 . C3 . H3 . 109.7 no
O31 . C3 . H3 . 109.9 no
C4 . C3 . H3 . 109.7 no
Na2 . O31 . C3 . 116.5(2) yes
Na2 . O31 . Mn1 . 102.07(16) yes
C3 . O31 . Mn1 . 109.8(7) yes
C3 . C4 . O41 . 119.5(7) yes
C3 . C4 . O42 . 114.6(4) yes
O41 . C4 . O42 . 125.8(4) yes
Na2 . O41 . Na3 1_565 107.57(15) yes
Na2 . O41 . C4 . 118.2(5) yes
Na3 1_565 O41 . C4 . 116.0(9) yes
H11 . O1 . H12 . 88.9 no
Na2 . O2 . H21 . 141.6 no
Na2 . O2 . H22 . 93.2 no
H21 . O2 . H22 . 103.5 no
Na2 . O3 . Na1 . 114.62(19) yes
Na2 . O3 . H31 . 97.4 no
Na1 . O3 . H31 . 103.9 no
Na2 . O3 . H32 . 93.0 no
Na1 . O3 . H32 . 119.6 no
H31 . O3 . H32 . 125.4 no
Na3 . O4 . Na2 . 121.69(18) yes
Na3 . O4 . H41 . 110.7 no
Na2 . O4 . H41 . 107.4 no
Na3 . O4 . H42 . 118.3 no
Na2 . O4 . H42 . 107.1 no
H41 . O4 . H42 . 85.3 no
Na1 . O5 . Na1 4_646 94.89(9) yes
Na1 . O5 . H51 . 101.3 no
Na1 4_646 O5 . H51 . 121.5 no
Na1 . O5 . H52 . 106.6 no
Na1 4_646 O5 . H52 . 106.4 no
H51 . O5 . H52 . 121.4 no
Na3 2_555 O6 . Na1 . 174.6(5) yes
Na3 2_555 O6 . H61 . 86.0 no
Na1 . O6 . H61 . 93.6 no
Na3 2_555 O6 . H62 . 90.0 no
Na1 . O6 . H62 . 85.5 no
H61 . O6 . H62 . 119.6 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1419434'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_6                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_6                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_6                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_6                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_6                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_6                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_6                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.9008(13)
_cell_length_b                   6.689(2)
_cell_length_c                   9.5275(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.453(3)
_cell_angle_gamma                90
_cell_volume                     1163.6(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.94 Fooo =    696.00 Mu =      7.72 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.94 FOOO =    696.00 Mu =      7.72 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.936
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.772

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4669
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1570
_diffrn_reflns_number            3716
_reflns_number_total             951
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 951 
# Number of reflections with Friedels Law is 600 
# Theoretical number of reflections is about 1190 


_diffrn_reflns_theta_min         2.825
_diffrn_reflns_theta_max         17.682
_diffrn_measured_fraction_theta_max 0.461

_diffrn_reflns_theta_full        15.207
_diffrn_measured_fraction_theta_full 0.472


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.51
_refine_diff_density_max         0.37


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         938
_refine_ls_number_restraints     82
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0426
_refine_ls_wR_factor_ref         0.0599
_refine_ls_goodness_of_fit_ref   0.9866
_refine_ls_shift/su_max          0.0003546
_refine_ls_shift/su_mean         0.0000422


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        938
_refine_ls_R_factor_all          0.0426
_refine_ls_wR_factor_all         0.0599

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                879
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_gt          0.0594

_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_abs_structure_details 'Flack (1983), 351 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8047(4) 0.0000 0.0217 1.0000 Uani S T . . . .
Na1 Na 0.73727(6) 0.5474(8) 0.49132(16) 0.0291 1.0000 Uani . . . . . .
Na2 Na 0.52243(6) 0.4936(7) 0.28563(13) 0.0301 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0244(9) 0.5000 0.0369 1.0000 Uani S T . . . .
C1 C 0.35177(14) 0.8304(18) -0.2112(3) 0.0238 1.0000 Uani . U . . . .
O11 O 0.28739(9) 0.7957(14) -0.3041(2) 0.0331 1.0000 Uani . U . . . .
O12 O 0.40836(10) 0.8120(14) -0.2416(2) 0.0248 1.0000 Uani . U . . . .
C2 C 0.36604(15) 0.8942(16) -0.0458(4) 0.0229 1.0000 Uani . U . . . .
O21 O 0.43399(10) 0.9933(13) 0.0205(2) 0.0266 1.0000 Uani . U . . . .
C3 C 0.37600(15) 0.6991(15) 0.0436(4) 0.0260 1.0000 Uani . U . . . .
O31 O 0.44193(11) 0.6082(12) 0.0487(2) 0.0263 1.0000 Uani . U . . . .
C4 C 0.37850(16) 0.7472(18) 0.2047(4) 0.0312 1.0000 Uani . U . . . .
O41 O 0.43349(12) 0.6980(12) 0.3203(2) 0.0286 1.0000 Uani . U . . . .
O42 O 0.32195(12) 0.8261(15) 0.2055(3) 0.0488 1.0000 Uani . U . . . .
O1 O 0.80949(12) 0.7897(16) 0.1535(3) 0.0554 1.0000 Uani . . . . . .
O2 O 0.57881(10) 0.3219(13) 0.1481(2) 0.0268 1.0000 Uani . U . . . .
O3 O 0.62479(12) 0.4544(12) 0.5090(2) 0.0295 1.0000 Uani . U . . . .
O4 O 0.45860(12) 0.1960(12) 0.2892(2) 0.0299 1.0000 Uani . U . . . .
O5 O 0.72039(9) 0.2862(13) 0.3231(2) 0.0319 1.0000 Uani . U . . . .
O6 O 0.87176(13) 0.5289(13) 0.4896(3) 0.0285 1.0000 Uani . U . . . .
H2 H 0.3251 0.9768 -0.0412 0.0273 1.0000 Uiso . . . . . .
H3 H 0.3336 0.6088 -0.0113 0.0310 1.0000 Uiso . . . . . .
H11 H 0.7807 0.7917 0.1983 0.0827 1.0000 Uiso . . . . . .
H12 H 0.8128 0.6659 0.1674 0.0827 1.0000 Uiso . . . . . .
H21 H 0.5748 0.2186 0.0950 0.0400 1.0000 Uiso . . . . . .
H22 H 0.5721 0.4146 0.0843 0.0400 1.0000 Uiso . . . . . .
H31 H 0.6258 0.3285 0.5095 0.0445 1.0000 Uiso . . . . . .
H32 H 0.6077 0.5258 0.5593 0.0445 1.0000 Uiso . . . . . .
H41 H 0.4511 0.1344 0.2074 0.0449 1.0000 Uiso . . . . . .
H42 H 0.4137 0.2243 0.2483 0.0449 1.0000 Uiso . . . . . .
H51 H 0.6755 0.2976 0.2677 0.0479 1.0000 Uiso . . . . . .
H52 H 0.7521 0.2988 0.2864 0.0479 1.0000 Uiso . . . . . .
H61 H 0.8570 0.4689 0.4053 0.0430 1.0000 Uiso . . . . . .
H62 H 0.8829 0.4634 0.5709 0.0430 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3638(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.2991(19) yes
Mn1 . O31 3_655 1.925(6) yes
Mn1 . O21 3_655 1.887(6) yes
Mn1 . O12 . 2.2991(19) yes
Mn1 . O21 . 1.887(6) yes
Mn1 . O31 . 1.925(6) yes
Na1 . O5 4_656 2.281(7) yes
Na1 . O11 3_655 2.342(8) yes
Na1 . O11 2_546 2.466(7) yes
Na1 . O3 . 2.393(3) yes
Na1 . O5 . 2.303(8) yes
Na1 . O6 . 2.686(3) yes
Na2 . O12 3_655 2.659(8) yes
Na2 . O31 . 2.318(4) yes
Na2 . O41 . 2.362(5) yes
Na2 . O2 . 2.338(5) yes
Na2 . O3 . 2.301(3) yes
Na2 . O4 . 2.369(7) yes
Na3 . O4 3_656 2.360(7) yes
Na3 . O41 1_545 2.515(8) yes
Na3 . O41 3_646 2.515(8) yes
Na3 . O6 2_445 2.539(3) yes
Na3 . O6 4_646 2.539(3) yes
Na3 . O4 . 2.360(7) yes
C1 . O11 . 1.255(4) yes
C1 . O12 . 1.276(4) yes
C1 . C2 . 1.546(6) yes
C2 . O21 . 1.410(7) yes
C2 . C3 . 1.527(14) yes
C2 . H2 . 1.000 no
C3 . O31 . 1.429(6) yes
C3 . C4 . 1.550(6) yes
C3 . H3 . 0.999 no
C4 . O41 . 1.249(6) yes
C4 . O42 . 1.246(7) yes
O1 . H11 . 0.840 no
O1 . H12 . 0.837 no
O2 . H21 . 0.841 no
O2 . H22 . 0.840 no
O3 . H31 . 0.842 no
O3 . H32 . 0.839 no
O4 . H41 . 0.840 no
O4 . H42 . 0.842 no
O5 . H51 . 0.840 no
O5 . H52 . 0.839 no
O6 . H61 . 0.839 no
O6 . H62 . 0.839 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.71(17) yes
O12 3_655 Mn1 . O21 3_655 77.42(18) yes
O31 3_655 Mn1 . O21 3_655 85.5(2) yes
O12 3_655 Mn1 . O12 . 177.6(5) yes
O31 3_655 Mn1 . O12 . 94.95(19) yes
O21 3_655 Mn1 . O12 . 100.93(19) yes
O12 3_655 Mn1 . O21 . 100.93(18) yes
O31 3_655 Mn1 . O21 . 172.36(10) yes
O21 3_655 Mn1 . O21 . 96.1(4) yes
O12 . Mn1 . O21 . 77.42(18) yes
O12 3_655 Mn1 . O31 . 94.95(19) yes
O31 3_655 Mn1 . O31 . 93.9(4) yes
O21 3_655 Mn1 . O31 . 172.36(10) yes
O12 . Mn1 . O31 . 86.71(17) yes
O21 . Mn1 . O31 . 85.5(2) yes
O5 4_656 Na1 . O11 3_655 89.7(3) yes
O5 4_656 Na1 . O11 2_546 87.54(19) yes
O11 3_655 Na1 . O11 2_546 169.26(9) yes
O5 4_656 Na1 . O3 . 101.24(16) yes
O11 3_655 Na1 . O3 . 108.64(16) yes
O11 2_546 Na1 . O3 . 82.08(17) yes
O5 4_656 Na1 . O5 . 167.75(15) yes
O11 3_655 Na1 . O5 . 94.57(19) yes
O11 2_546 Na1 . O5 . 86.2(3) yes
O3 . Na1 . O5 . 88.29(19) yes
O5 4_656 Na1 . O6 . 88.60(16) yes
O11 3_655 Na1 . O6 . 86.29(17) yes
O11 2_546 Na1 . O6 . 83.27(16) yes
O3 . Na1 . O6 . 161.9(4) yes
O5 . Na1 . O6 . 80.24(17) yes
O12 3_655 Na2 . O31 . 77.41(19) yes
O12 3_655 Na2 . O41 . 91.3(2) yes
O31 . Na2 . O41 . 71.27(15) yes
O12 3_655 Na2 . O2 . 84.9(2) yes
O31 . Na2 . O2 . 85.20(16) yes
O41 . Na2 . O2 . 156.42(12) yes
O12 3_655 Na2 . O3 . 85.06(19) yes
O31 . Na2 . O3 . 162.3(3) yes
O41 . Na2 . O3 . 111.93(16) yes
O2 . Na2 . O3 . 90.96(14) yes
O12 3_655 Na2 . O4 . 171.81(13) yes
O31 . Na2 . O4 . 97.2(2) yes
O41 . Na2 . O4 . 92.78(19) yes
O2 . Na2 . O4 . 88.6(2) yes
O3 . Na2 . O4 . 100.0(2) yes
O4 3_656 Na3 . O41 1_545 162.04(17) yes
O4 3_656 Na3 . O41 3_646 88.34(18) yes
O41 1_545 Na3 . O41 3_646 84.8(3) yes
O4 3_656 Na3 . O6 2_445 87.17(17) yes
O41 1_545 Na3 . O6 2_445 80.13(19) yes
O41 3_646 Na3 . O6 2_445 112.26(19) yes
O4 3_656 Na3 . O6 4_646 82.76(16) yes
O41 1_545 Na3 . O6 4_646 112.26(19) yes
O41 3_646 Na3 . O6 4_646 80.13(19) yes
O6 2_445 Na3 . O6 4_646 163.9(5) yes
O4 3_656 Na3 . O4 . 102.7(4) yes
O41 1_545 Na3 . O4 . 88.34(18) yes
O41 3_646 Na3 . O4 . 162.04(17) yes
O6 2_445 Na3 . O4 . 82.76(16) yes
O6 4_646 Na3 . O4 . 87.17(17) yes
O11 . C1 . O12 . 124.6(4) yes
O11 . C1 . C2 . 119.4(3) yes
O12 . C1 . C2 . 116.0(3) yes
Na1 3_655 O11 . Na1 2_454 89.19(6) yes
Na1 3_655 O11 . C1 . 120.9(6) yes
Na1 2_454 O11 . C1 . 114.2(7) yes
Mn1 . O12 . C1 . 101.23(16) yes
Mn1 . O12 . Na2 3_655 83.49(19) yes
C1 . O12 . Na2 3_655 132.3(7) yes
C1 . C2 . O21 . 109.9(3) yes
C1 . C2 . C3 . 105.2(8) yes
O21 . C2 . C3 . 105.3(4) yes
C1 . C2 . H2 . 112.0 no
O21 . C2 . H2 . 112.0 no
C3 . C2 . H2 . 112.0 no
C2 . O21 . Mn1 . 102.8(6) yes
C2 . C3 . O31 . 107.2(4) yes
C2 . C3 . C4 . 108.7(8) yes
O31 . C3 . C4 . 112.8(3) yes
C2 . C3 . H3 . 109.3 no
O31 . C3 . H3 . 109.5 no
C4 . C3 . H3 . 109.4 no
Na2 . O31 . C3 . 116.30(19) yes
Na2 . O31 . Mn1 . 102.24(14) yes
C3 . O31 . Mn1 . 109.4(6) yes
C3 . C4 . O41 . 119.4(5) yes
C3 . C4 . O42 . 114.9(3) yes
O41 . C4 . O42 . 125.6(4) yes
Na2 . O41 . Na3 1_565 107.57(12) yes
Na2 . O41 . C4 . 118.1(4) yes
Na3 1_565 O41 . C4 . 116.4(8) yes
H11 . O1 . H12 . 87.9 no
Na2 . O2 . H21 . 142.1 no
Na2 . O2 . H22 . 94.0 no
H21 . O2 . H22 . 102.8 no
Na2 . O3 . Na1 . 114.44(16) yes
Na2 . O3 . H31 . 97.5 no
Na1 . O3 . H31 . 103.8 no
Na2 . O3 . H32 . 93.0 no
Na1 . O3 . H32 . 119.7 no
H31 . O3 . H32 . 125.5 no
Na3 . O4 . Na2 . 121.97(16) yes
Na3 . O4 . H41 . 110.9 no
Na2 . O4 . H41 . 107.3 no
Na3 . O4 . H42 . 118.7 no
Na2 . O4 . H42 . 106.3 no
H41 . O4 . H42 . 85.2 no
Na1 . O5 . Na1 4_646 94.90(7) yes
Na1 . O5 . H51 . 101.1 no
Na1 4_646 O5 . H51 . 121.5 no
Na1 . O5 . H52 . 106.8 no
Na1 4_646 O5 . H52 . 106.6 no
H51 . O5 . H52 . 121.1 no
Na3 2_555 O6 . Na1 . 174.1(4) yes
Na3 2_555 O6 . H61 . 86.2 no
Na1 . O6 . H61 . 93.3 no
Na3 2_555 O6 . H62 . 90.0 no
Na1 . O6 . H62 . 85.1 no
H61 . O6 . H62 . 119.8 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7
_database_code_depnum_ccdc_archive 'CCDC 1419435'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_7                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_7                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_7                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_7                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_7                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_7                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_7                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.8482(14)
_cell_length_b                   6.664(2)
_cell_length_c                   9.5173(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.535(4)
_cell_angle_gamma                90
_cell_volume                     1154.1(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.95 Fooo =    696.00 Mu =      7.78 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.95 FOOO =    696.00 Mu =      7.78 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.778

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4776
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         1800
_diffrn_reflns_number            3968
_reflns_number_total             982
_diffrn_reflns_av_R_equivalents  0.047
# Number of reflections without Friedels Law is 982 
# Number of reflections with Friedels Law is 617 
# Theoretical number of reflections is about 1181 


_diffrn_reflns_theta_min         1.596
_diffrn_reflns_theta_max         17.682
_diffrn_measured_fraction_theta_max 0.476

_diffrn_reflns_theta_full        15.383
_diffrn_measured_fraction_theta_full 0.488


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.31
_refine_diff_density_max         1.09


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         966
_refine_ls_number_restraints     142
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0569
_refine_ls_wR_factor_ref         0.0611
_refine_ls_goodness_of_fit_ref   0.9978
_refine_ls_shift/su_max          0.0002815
_refine_ls_shift/su_mean         0.0000459


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        966
_refine_ls_R_factor_all          0.0569
_refine_ls_wR_factor_all         0.0611

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                853
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_gt          0.0586

_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_abs_structure_details 'Flack (1983), 365 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8049(4) 0.0000 0.0231 1.0000 Uani S T . . . .
Na1 Na 0.73707(7) 0.5462(9) 0.49130(18) 0.0261 1.0000 Uani . . . . . .
Na2 Na 0.52228(7) 0.4944(8) 0.28623(14) 0.0335 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0250(10) 0.5000 0.0413 1.0000 Uani S T . . . .
C1 C 0.35127(15) 0.833(2) -0.2122(3) 0.0260 1.0000 Uani . U . . . .
O11 O 0.28692(10) 0.7996(16) -0.3048(2) 0.0344 1.0000 Uani . U . . . .
O12 O 0.40823(11) 0.8129(16) -0.2425(2) 0.0258 1.0000 Uani . U . . . .
C2 C 0.36594(17) 0.8955(18) -0.0460(4) 0.0241 1.0000 Uani . U . . . .
O21 O 0.43365(11) 0.9927(14) 0.0205(3) 0.0270 1.0000 Uani . U . . . .
C3 C 0.37537(16) 0.6978(18) 0.0428(4) 0.0267 1.0000 Uani . U . . . .
O31 O 0.44177(12) 0.6088(13) 0.0487(3) 0.0268 1.0000 Uani . U . . . .
C4 C 0.37756(17) 0.750(2) 0.2030(4) 0.0301 1.0000 Uani . U . . . .
O41 O 0.43302(13) 0.6989(13) 0.3203(3) 0.0305 1.0000 Uani . U . . . .
O42 O 0.32058(14) 0.8232(17) 0.2038(3) 0.0476 1.0000 Uani . U . . . .
O1 O 0.80924(13) 0.7942(19) 0.1520(3) 0.0600 1.0000 Uani . . . . . .
O2 O 0.57861(11) 0.3203(15) 0.1491(3) 0.0285 1.0000 Uani . U . . . .
O3 O 0.62478(13) 0.4531(14) 0.5091(3) 0.0304 1.0000 Uani . U . . . .
O4 O 0.45832(12) 0.1925(13) 0.2890(3) 0.0321 1.0000 Uani . U . . . .
O5 O 0.72004(10) 0.2861(15) 0.3232(2) 0.0335 1.0000 Uani . U . . . .
O6 O 0.87146(15) 0.5270(15) 0.4886(3) 0.0284 1.0000 Uani . U . . . .
H2 H 0.3250 0.9786 -0.0412 0.0287 1.0000 Uiso . . . . . .
H3 H 0.3329 0.6071 -0.0122 0.0318 1.0000 Uiso . . . . . .
H11 H 0.7806 0.7963 0.1973 0.0867 1.0000 Uiso . . . . . .
H12 H 0.8122 0.6702 0.1656 0.0867 1.0000 Uiso . . . . . .
H21 H 0.5748 0.2171 0.0955 0.0426 1.0000 Uiso . . . . . .
H22 H 0.5720 0.4133 0.0851 0.0426 1.0000 Uiso . . . . . .
H31 H 0.6259 0.3267 0.5099 0.0461 1.0000 Uiso . . . . . .
H32 H 0.6077 0.5252 0.5595 0.0461 1.0000 Uiso . . . . . .
H41 H 0.4507 0.1314 0.2068 0.0481 1.0000 Uiso . . . . . .
H42 H 0.4135 0.2233 0.2478 0.0481 1.0000 Uiso . . . . . .
H51 H 0.6750 0.2971 0.2677 0.0503 1.0000 Uiso . . . . . .
H52 H 0.7516 0.2979 0.2857 0.0503 1.0000 Uiso . . . . . .
H61 H 0.8564 0.4671 0.4042 0.0429 1.0000 Uiso . . . . . .
H62 H 0.8826 0.4623 0.5703 0.0429 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2917(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.300(2) yes
Mn1 . O31 3_655 1.920(7) yes
Mn1 . O21 3_655 1.883(7) yes
Mn1 . O12 . 2.300(2) yes
Mn1 . O21 . 1.883(7) yes
Mn1 . O31 . 1.920(7) yes
Na1 . O5 4_656 2.280(9) yes
Na1 . O11 3_655 2.357(9) yes
Na1 . O11 2_546 2.431(9) yes
Na1 . O3 . 2.384(4) yes
Na1 . O5 . 2.290(9) yes
Na1 . O6 . 2.681(3) yes
Na2 . O12 3_655 2.653(9) yes
Na2 . O31 . 2.316(4) yes
Na2 . O41 . 2.358(6) yes
Na2 . O2 . 2.338(6) yes
Na2 . O3 . 2.295(3) yes
Na2 . O4 . 2.385(8) yes
Na3 . O4 3_656 2.343(7) yes
Na3 . O41 1_545 2.502(9) yes
Na3 . O41 3_646 2.502(9) yes
Na3 . O6 2_445 2.534(3) yes
Na3 . O6 4_646 2.534(3) yes
Na3 . O4 . 2.343(7) yes
C1 . O11 . 1.248(5) yes
C1 . O12 . 1.280(4) yes
C1 . C2 . 1.547(7) yes
C2 . O21 . 1.395(8) yes
C2 . C3 . 1.536(17) yes
C2 . H2 . 0.999 no
C3 . O31 . 1.426(7) yes
C3 . C4 . 1.547(6) yes
C3 . H3 . 0.998 no
C4 . O41 . 1.261(6) yes
C4 . O42 . 1.235(7) yes
O1 . H11 . 0.840 no
O1 . H12 . 0.835 no
O2 . H21 . 0.841 no
O2 . H22 . 0.842 no
O3 . H31 . 0.843 no
O3 . H32 . 0.839 no
O4 . H41 . 0.840 no
O4 . H42 . 0.842 no
O5 . H51 . 0.841 no
O5 . H52 . 0.839 no
O6 . H61 . 0.838 no
O6 . H62 . 0.838 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 86.9(2) yes
O12 3_655 Mn1 . O21 3_655 77.4(2) yes
O31 3_655 Mn1 . O21 3_655 85.1(2) yes
O12 3_655 Mn1 . O12 . 177.4(6) yes
O31 3_655 Mn1 . O12 . 94.9(2) yes
O21 3_655 Mn1 . O12 . 100.8(2) yes
O12 3_655 Mn1 . O21 . 100.8(2) yes
O31 3_655 Mn1 . O21 . 172.31(12) yes
O21 3_655 Mn1 . O21 . 96.7(4) yes
O12 . Mn1 . O21 . 77.4(2) yes
O12 3_655 Mn1 . O31 . 94.9(2) yes
O31 3_655 Mn1 . O31 . 94.2(4) yes
O21 3_655 Mn1 . O31 . 172.31(12) yes
O12 . Mn1 . O31 . 86.9(2) yes
O21 . Mn1 . O31 . 85.1(2) yes
O5 4_656 Na1 . O11 3_655 88.9(4) yes
O5 4_656 Na1 . O11 2_546 87.1(2) yes
O11 3_655 Na1 . O11 2_546 168.77(14) yes
O5 4_656 Na1 . O3 . 101.42(19) yes
O11 3_655 Na1 . O3 . 109.06(19) yes
O11 2_546 Na1 . O3 . 82.0(2) yes
O5 4_656 Na1 . O5 . 167.67(16) yes
O11 3_655 Na1 . O5 . 95.0(2) yes
O11 2_546 Na1 . O5 . 86.9(4) yes
O3 . Na1 . O5 . 88.4(2) yes
O5 4_656 Na1 . O6 . 88.61(19) yes
O11 3_655 Na1 . O6 . 85.96(19) yes
O11 2_546 Na1 . O6 . 83.46(19) yes
O3 . Na1 . O6 . 161.9(4) yes
O5 . Na1 . O6 . 80.0(2) yes
O12 3_655 Na2 . O31 . 77.4(2) yes
O12 3_655 Na2 . O41 . 91.5(3) yes
O31 . Na2 . O41 . 71.36(17) yes
O12 3_655 Na2 . O2 . 85.1(3) yes
O31 . Na2 . O2 . 85.16(18) yes
O41 . Na2 . O2 . 156.44(13) yes
O12 3_655 Na2 . O3 . 85.2(2) yes
O31 . Na2 . O3 . 162.4(3) yes
O41 . Na2 . O3 . 112.31(19) yes
O2 . Na2 . O3 . 90.67(16) yes
O12 3_655 Na2 . O4 . 171.51(15) yes
O31 . Na2 . O4 . 97.2(2) yes
O41 . Na2 . O4 . 93.1(2) yes
O2 . Na2 . O4 . 87.9(3) yes
O3 . Na2 . O4 . 99.7(3) yes
O4 3_656 Na3 . O41 1_545 161.80(19) yes
O4 3_656 Na3 . O41 3_646 87.7(2) yes
O41 1_545 Na3 . O41 3_646 85.4(4) yes
O4 3_656 Na3 . O6 2_445 87.5(2) yes
O41 1_545 Na3 . O6 2_445 79.6(2) yes
O41 3_646 Na3 . O6 2_445 112.4(2) yes
O4 3_656 Na3 . O6 4_646 82.74(19) yes
O41 1_545 Na3 . O6 4_646 112.4(2) yes
O41 3_646 Na3 . O6 4_646 79.6(2) yes
O6 2_445 Na3 . O6 4_646 164.3(6) yes
O4 3_656 Na3 . O4 . 103.6(4) yes
O41 1_545 Na3 . O4 . 87.7(2) yes
O41 3_646 Na3 . O4 . 161.80(19) yes
O6 2_445 Na3 . O4 . 82.74(19) yes
O6 4_646 Na3 . O4 . 87.5(2) yes
O11 . C1 . O12 . 124.7(4) yes
O11 . C1 . C2 . 119.4(3) yes
O12 . C1 . C2 . 115.8(3) yes
Na1 3_655 O11 . Na1 2_454 89.30(7) yes
Na1 3_655 O11 . C1 . 120.0(7) yes
Na1 2_454 O11 . C1 . 114.8(8) yes
Mn1 . O12 . C1 . 101.15(18) yes
Mn1 . O12 . Na2 3_655 83.5(2) yes
C1 . O12 . Na2 3_655 132.8(8) yes
C1 . C2 . O21 . 110.1(3) yes
C1 . C2 . C3 . 105.2(9) yes
O21 . C2 . C3 . 105.4(5) yes
C1 . C2 . H2 . 111.9 no
O21 . C2 . H2 . 112.0 no
C3 . C2 . H2 . 111.9 no
C2 . O21 . Mn1 . 103.4(7) yes
C2 . C3 . O31 . 106.6(5) yes
C2 . C3 . C4 . 107.5(10) yes
O31 . C3 . C4 . 113.1(4) yes
C2 . C3 . H3 . 109.8 no
O31 . C3 . H3 . 110.0 no
C4 . C3 . H3 . 109.7 no
Na2 . O31 . C3 . 116.2(2) yes
Na2 . O31 . Mn1 . 102.27(15) yes
C3 . O31 . Mn1 . 110.1(7) yes
C3 . C4 . O41 . 118.9(6) yes
C3 . C4 . O42 . 115.4(4) yes
O41 . C4 . O42 . 125.4(4) yes
Na2 . O41 . Na3 1_565 107.19(13) yes
Na2 . O41 . C4 . 118.2(5) yes
Na3 1_565 O41 . C4 . 116.4(9) yes
H11 . O1 . H12 . 87.6 no
Na2 . O2 . H21 . 142.8 no
Na2 . O2 . H22 . 93.9 no
H21 . O2 . H22 . 102.3 no
Na2 . O3 . Na1 . 114.32(18) yes
Na2 . O3 . H31 . 98.0 no
Na1 . O3 . H31 . 103.8 no
Na2 . O3 . H32 . 92.8 no
Na1 . O3 . H32 . 119.5 no
H31 . O3 . H32 . 125.6 no
Na3 . O4 . Na2 . 121.61(17) yes
Na3 . O4 . H41 . 111.6 no
Na2 . O4 . H41 . 107.3 no
Na3 . O4 . H42 . 119.8 no
Na2 . O4 . H42 . 104.9 no
H41 . O4 . H42 . 85.4 no
Na1 . O5 . Na1 4_646 94.85(8) yes
Na1 . O5 . H51 . 101.3 no
Na1 4_646 O5 . H51 . 121.5 no
Na1 . O5 . H52 . 107.4 no
Na1 4_646 O5 . H52 . 106.5 no
H51 . O5 . H52 . 120.8 no
Na3 2_555 O6 . Na1 . 174.2(4) yes
Na3 2_555 O6 . H61 . 86.8 no
Na1 . O6 . H61 . 93.2 no
Na3 2_555 O6 . H62 . 90.0 no
Na1 . O6 . H62 . 84.9 no
H61 . O6 . H62 . 120.4 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1419436'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_8                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_8                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_8                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_8                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_8                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_8                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_8                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.7638(18)
_cell_length_b                   6.621(3)
_cell_length_c                   9.5007(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.677(5)
_cell_angle_gamma                90
_cell_volume                     1138.6(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.98 Fooo =    696.00 Mu =      7.89 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      1.98 FOOO =    696.00 Mu =      7.89 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.789

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4864
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         2290
_diffrn_reflns_number            3915
_reflns_number_total             965
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 965 
# Number of reflections with Friedels Law is 608 
# Theoretical number of reflections is about 1166 


_diffrn_reflns_theta_min         1.600
_diffrn_reflns_theta_max         17.686
_diffrn_measured_fraction_theta_max 0.478

_diffrn_reflns_theta_full        15.033
_diffrn_measured_fraction_theta_full 0.489


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.68
_refine_diff_density_max         0.56


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         955
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0452
_refine_ls_wR_factor_ref         0.0579
_refine_ls_goodness_of_fit_ref   1.0006
_refine_ls_shift/su_max          0.0002611
_refine_ls_shift/su_mean         0.0000261


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        955
_refine_ls_R_factor_all          0.0452
_refine_ls_wR_factor_all         0.0579

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                874
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_gt          0.0567

_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_abs_structure_details 'Flack (1983), 357 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8048(4) 0.0000 0.0212 1.0000 Uani S T . . . .
Na1 Na 0.73686(7) 0.5439(8) 0.49120(17) 0.0297 1.0000 Uani . . . . . .
Na2 Na 0.52201(6) 0.4951(7) 0.28738(13) 0.0317 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0244(9) 0.5000 0.0357 1.0000 Uani S T . . . .
C1 C 0.35084(15) 0.8340(18) -0.2133(3) 0.0213 1.0000 Uani . U . . . .
O11 O 0.28635(10) 0.7958(14) -0.3056(2) 0.0314 1.0000 Uani . U . . . .
O12 O 0.40819(10) 0.8139(14) -0.2431(2) 0.0242 1.0000 Uani . U . . . .
C2 C 0.36542(16) 0.8963(16) -0.0473(4) 0.0198 1.0000 Uani . U . . . .
O21 O 0.43364(11) 0.9953(13) 0.0206(2) 0.0229 1.0000 Uani . U . . . .
C3 C 0.37462(15) 0.6970(17) 0.0416(4) 0.0219 1.0000 Uani . U . . . .
O31 O 0.44147(11) 0.6080(12) 0.0489(2) 0.0231 1.0000 Uani . U . . . .
C4 C 0.37669(16) 0.749(2) 0.2025(4) 0.0249 1.0000 Uani . U . . . .
O41 O 0.43215(12) 0.6993(12) 0.3195(2) 0.0267 1.0000 Uani . U . . . .
O42 O 0.31887(13) 0.8246(16) 0.2009(3) 0.0478 1.0000 Uani . U . . . .
O1 O 0.80911(12) 0.7968(17) 0.1499(3) 0.0504 1.0000 Uani . . . . . .
O2 O 0.57779(10) 0.3222(13) 0.1496(2) 0.0273 1.0000 Uani . U . . . .
O3 O 0.62460(12) 0.4517(13) 0.5100(3) 0.0285 1.0000 Uani . U . . . .
O4 O 0.45819(11) 0.1936(12) 0.2898(2) 0.0283 1.0000 Uani . U . . . .
O5 O 0.71962(10) 0.2820(14) 0.3236(2) 0.0307 1.0000 Uani . U . . . .
O6 O 0.87104(14) 0.5270(14) 0.4874(3) 0.0263 1.0000 Uani . U . . . .
H2 H 0.3238 0.9742 -0.0431 0.0321 1.0000 Uiso . . . . . .
H3 H 0.3330 0.6036 -0.0141 0.0332 1.0000 Uiso . . . . . .
H11 H 0.7811 0.8003 0.1968 0.0765 1.0000 Uiso . . . . . .
H12 H 0.8123 0.6750 0.1644 0.0765 1.0000 Uiso . . . . . .
H21 H 0.5742 0.2178 0.0961 0.0507 1.0000 Uiso . . . . . .
H22 H 0.5717 0.4138 0.0859 0.0507 1.0000 Uiso . . . . . .
H31 H 0.6259 0.3287 0.5099 0.0513 1.0000 Uiso . . . . . .
H32 H 0.6077 0.5277 0.5601 0.0513 1.0000 Uiso . . . . . .
H41 H 0.4506 0.1322 0.2069 0.0512 1.0000 Uiso . . . . . .
H42 H 0.4132 0.2257 0.2475 0.0512 1.0000 Uiso . . . . . .
H51 H 0.6742 0.2927 0.2679 0.0523 1.0000 Uiso . . . . . .
H52 H 0.7508 0.2943 0.2850 0.0523 1.0000 Uiso . . . . . .
H61 H 0.8557 0.4663 0.4027 0.0487 1.0000 Uiso . . . . . .
H62 H 0.8825 0.4606 0.5704 0.0487 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3059(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.2944(19) yes
Mn1 . O31 3_655 1.919(6) yes
Mn1 . O21 3_655 1.886(6) yes
Mn1 . O12 . 2.2944(19) yes
Mn1 . O21 . 1.886(6) yes
Mn1 . O31 . 1.919(6) yes
Na1 . O11 3_655 2.335(8) yes
Na1 . O5 4_656 2.260(8) yes
Na1 . O11 2_546 2.422(8) yes
Na1 . O3 . 2.376(3) yes
Na1 . O5 . 2.285(8) yes
Na1 . O6 . 2.669(3) yes
Na2 . O12 3_655 2.646(8) yes
Na2 . O31 . 2.309(4) yes
Na2 . O41 . 2.348(6) yes
Na2 . O2 . 2.323(5) yes
Na2 . O3 . 2.285(3) yes
Na2 . O4 . 2.366(8) yes
Na3 . O4 3_656 2.330(7) yes
Na3 . O41 1_545 2.498(8) yes
Na3 . O41 3_646 2.498(8) yes
Na3 . O6 2_445 2.526(3) yes
Na3 . O6 4_646 2.526(3) yes
Na3 . O4 . 2.330(7) yes
C1 . O11 . 1.249(5) yes
C1 . O12 . 1.280(4) yes
C1 . C2 . 1.541(6) yes
C2 . O21 . 1.402(7) yes
C2 . C3 . 1.538(15) yes
C2 . H2 . 0.986 no
C3 . O31 . 1.423(7) yes
C3 . C4 . 1.550(6) yes
C3 . H3 . 0.995 no
C4 . O41 . 1.251(6) yes
C4 . O42 . 1.243(7) yes
O1 . H11 . 0.839 no
O1 . H12 . 0.816 no
O2 . H21 . 0.844 no
O2 . H22 . 0.831 no
O3 . H31 . 0.815 no
O3 . H32 . 0.847 no
O4 . H41 . 0.844 no
O4 . H42 . 0.843 no
O5 . H51 . 0.842 no
O5 . H52 . 0.838 no
O6 . H61 . 0.840 no
O6 . H62 . 0.851 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 87.23(18) yes
O12 3_655 Mn1 . O21 3_655 77.57(19) yes
O31 3_655 Mn1 . O21 3_655 85.24(19) yes
O12 3_655 Mn1 . O12 . 177.0(5) yes
O31 3_655 Mn1 . O12 . 94.84(19) yes
O21 3_655 Mn1 . O12 . 100.35(19) yes
O12 3_655 Mn1 . O21 . 100.35(19) yes
O31 3_655 Mn1 . O21 . 172.41(10) yes
O21 3_655 Mn1 . O21 . 96.0(4) yes
O12 . Mn1 . O21 . 77.57(19) yes
O12 3_655 Mn1 . O31 . 94.84(19) yes
O31 3_655 Mn1 . O31 . 94.5(4) yes
O21 3_655 Mn1 . O31 . 172.41(10) yes
O12 . Mn1 . O31 . 87.23(18) yes
O21 . Mn1 . O31 . 85.24(19) yes
O11 3_655 Na1 . O5 4_656 89.3(3) yes
O11 3_655 Na1 . O11 2_546 168.65(11) yes
O5 4_656 Na1 . O11 2_546 86.96(19) yes
O11 3_655 Na1 . O3 . 109.52(17) yes
O5 4_656 Na1 . O3 . 101.29(17) yes
O11 2_546 Na1 . O3 . 81.73(18) yes
O11 3_655 Na1 . O5 . 94.97(19) yes
O5 4_656 Na1 . O5 . 167.31(16) yes
O11 2_546 Na1 . O5 . 86.6(3) yes
O3 . Na1 . O5 . 88.6(2) yes
O11 3_655 Na1 . O6 . 85.10(18) yes
O5 4_656 Na1 . O6 . 88.29(17) yes
O11 2_546 Na1 . O6 . 84.09(17) yes
O3 . Na1 . O6 . 162.4(4) yes
O5 . Na1 . O6 . 80.19(18) yes
O12 3_655 Na2 . O31 . 77.5(2) yes
O12 3_655 Na2 . O41 . 91.8(2) yes
O31 . Na2 . O41 . 71.44(15) yes
O12 3_655 Na2 . O2 . 84.7(2) yes
O31 . Na2 . O2 . 84.42(17) yes
O41 . Na2 . O2 . 155.78(12) yes
O12 3_655 Na2 . O3 . 85.5(2) yes
O31 . Na2 . O3 . 162.7(3) yes
O41 . Na2 . O3 . 112.85(17) yes
O2 . Na2 . O3 . 90.82(15) yes
O12 3_655 Na2 . O4 . 171.27(14) yes
O31 . Na2 . O4 . 97.0(2) yes
O41 . Na2 . O4 . 92.89(19) yes
O2 . Na2 . O4 . 88.0(3) yes
O3 . Na2 . O4 . 99.4(2) yes
O4 3_656 Na3 . O41 1_545 161.79(17) yes
O4 3_656 Na3 . O41 3_646 87.57(18) yes
O41 1_545 Na3 . O41 3_646 85.8(3) yes
O4 3_656 Na3 . O6 2_445 87.77(18) yes
O41 1_545 Na3 . O6 2_445 79.2(2) yes
O41 3_646 Na3 . O6 2_445 112.6(2) yes
O4 3_656 Na3 . O6 4_646 82.66(17) yes
O41 1_545 Na3 . O6 4_646 112.6(2) yes
O41 3_646 Na3 . O6 4_646 79.2(2) yes
O6 2_445 Na3 . O6 4_646 164.5(5) yes
O4 3_656 Na3 . O4 . 103.5(4) yes
O41 1_545 Na3 . O4 . 87.57(18) yes
O41 3_646 Na3 . O4 . 161.79(17) yes
O6 2_445 Na3 . O4 . 82.66(17) yes
O6 4_646 Na3 . O4 . 87.77(18) yes
O11 . C1 . O12 . 124.7(4) yes
O11 . C1 . C2 . 119.4(3) yes
O12 . C1 . C2 . 115.8(3) yes
Na1 3_655 O11 . Na1 2_454 89.33(7) yes
Na1 3_655 O11 . C1 . 120.7(6) yes
Na1 2_454 O11 . C1 . 113.2(7) yes
Mn1 . O12 . C1 . 101.12(17) yes
Mn1 . O12 . Na2 3_655 83.5(2) yes
C1 . O12 . Na2 3_655 133.0(7) yes
C1 . C2 . O21 . 110.3(3) yes
C1 . C2 . C3 . 105.4(8) yes
O21 . C2 . C3 . 105.6(4) yes
C1 . C2 . H2 . 111.4 no
O21 . C2 . H2 . 113.7 no
C3 . C2 . H2 . 110.1 no
C2 . O21 . Mn1 . 102.7(6) yes
C2 . C3 . O31 . 106.5(4) yes
C2 . C3 . C4 . 107.6(9) yes
O31 . C3 . C4 . 112.8(3) yes
C2 . C3 . H3 . 110.5 no
O31 . C3 . H3 . 108.7 no
C4 . C3 . H3 . 110.5 no
Na2 . O31 . C3 . 116.26(19) yes
Na2 . O31 . Mn1 . 102.26(14) yes
C3 . O31 . Mn1 . 110.2(6) yes
C3 . C4 . O41 . 119.1(6) yes
C3 . C4 . O42 . 114.6(3) yes
O41 . C4 . O42 . 126.1(4) yes
Na2 . O41 . Na3 1_565 106.59(12) yes
Na2 . O41 . C4 . 118.2(4) yes
Na3 1_565 O41 . C4 . 117.1(8) yes
H11 . O1 . H12 . 87.6 no
Na2 . O2 . H21 . 143.0 no
Na2 . O2 . H22 . 95.0 no
H21 . O2 . H22 . 102.0 no
Na2 . O3 . Na1 . 113.96(17) yes
Na2 . O3 . H31 . 98.1 no
Na1 . O3 . H31 . 103.0 no
Na2 . O3 . H32 . 92.4 no
Na1 . O3 . H32 . 118.6 no
H31 . O3 . H32 . 127.9 no
Na3 . O4 . Na2 . 121.59(16) yes
Na3 . O4 . H41 . 111.7 no
Na2 . O4 . H41 . 107.1 no
Na3 . O4 . H42 . 120.5 no
Na2 . O4 . H42 . 104.3 no
H41 . O4 . H42 . 85.3 no
Na1 . O5 . Na1 4_646 94.78(8) yes
Na1 . O5 . H51 . 101.4 no
Na1 4_646 O5 . H51 . 121.6 no
Na1 . O5 . H52 . 107.5 no
Na1 4_646 O5 . H52 . 107.0 no
H51 . O5 . H52 . 120.1 no
Na3 2_555 O6 . Na1 . 173.8(4) yes
Na3 2_555 O6 . H61 . 87.2 no
Na1 . O6 . H61 . 93.1 no
Na3 2_555 O6 . H62 . 90.0 no
Na1 . O6 . H62 . 84.5 no
H61 . O6 . H62 . 120.0 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 1419437'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_9                   
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_9                   
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_9                   
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_9                   
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_9                   
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_9                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_9                   
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.6986(13)
_cell_length_b                   6.5700(18)
_cell_length_c                   9.4982(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.778(4)
_cell_angle_gamma                90
_cell_volume                     1124.9(3)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.00 Fooo =    696.00 Mu =      7.98 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.00 FOOO =    696.00 Mu =      7.98 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.798

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.5144
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         2650
_diffrn_reflns_number            3814
_reflns_number_total             969
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 969 
# Number of reflections with Friedels Law is 615 
# Theoretical number of reflections is about 1139 


_diffrn_reflns_theta_min         1.602
_diffrn_reflns_theta_max         17.616
_diffrn_measured_fraction_theta_max 0.495

_diffrn_reflns_theta_full        14.974
_diffrn_measured_fraction_theta_full 0.503


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.16
_refine_diff_density_max         1.22


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         962
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0554
_refine_ls_wR_factor_ref         0.0633
_refine_ls_goodness_of_fit_ref   0.9994
_refine_ls_shift/su_max          0.0005730
_refine_ls_shift/su_mean         0.0000618


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        962
_refine_ls_R_factor_all          0.0554
_refine_ls_wR_factor_all         0.0633

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                858
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_gt          0.0620

_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_abs_structure_details 'Flack (1983), 354 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8045(5) 0.0000 0.0251 1.0000 Uani S T . . . .
Na1 Na 0.73669(8) 0.5446(10) 0.49106(19) 0.0267 1.0000 Uani . . . . . .
Na2 Na 0.52185(7) 0.4974(8) 0.28798(16) 0.0330 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0247(11) 0.5000 0.0306 1.0000 Uani S T . . . .
C1 C 0.35046(17) 0.833(2) -0.2128(4) 0.0245 1.0000 Uani . U . . . .
O11 O 0.28577(11) 0.7953(17) -0.3062(2) 0.0325 1.0000 Uani . U . . . .
O12 O 0.40800(11) 0.8148(17) -0.2435(2) 0.0262 1.0000 Uani . U . . . .
C2 C 0.36494(18) 0.897(2) -0.0482(4) 0.0243 1.0000 Uani . U . . . .
O21 O 0.43358(12) 0.9967(15) 0.0204(3) 0.0263 1.0000 Uani . U . . . .
C3 C 0.37394(18) 0.697(2) 0.0407(4) 0.0256 1.0000 Uani . U . . . .
O31 O 0.44113(12) 0.6054(14) 0.0491(3) 0.0265 1.0000 Uani . U . . . .
C4 C 0.37533(19) 0.747(2) 0.2006(4) 0.0313 1.0000 Uani . U . . . .
O41 O 0.43132(13) 0.6974(14) 0.3191(3) 0.0285 1.0000 Uani . U . . . .
O42 O 0.31746(15) 0.8228(18) 0.1987(3) 0.0489 1.0000 Uani . U . . . .
O1 O 0.80892(14) 0.798(2) 0.1491(3) 0.0575 1.0000 Uani . . . . . .
O2 O 0.57719(12) 0.3228(15) 0.1511(3) 0.0283 1.0000 Uani . U . . . .
O3 O 0.62475(14) 0.4531(15) 0.5104(3) 0.0315 1.0000 Uani . U . . . .
O4 O 0.45781(13) 0.1947(14) 0.2901(3) 0.0301 1.0000 Uani . U . . . .
O5 O 0.71912(11) 0.2804(16) 0.3231(2) 0.0320 1.0000 Uani . U . . . .
O6 O 0.87078(15) 0.5270(16) 0.4874(3) 0.0282 1.0000 Uani . U . . . .
H2 H 0.3233 0.9736 -0.0439 0.0458 1.0000 Uiso . . . . . .
H3 H 0.3319 0.6005 -0.0168 0.0464 1.0000 Uiso . . . . . .
H11 H 0.7809 0.8027 0.1974 0.0771 1.0000 Uiso . . . . . .
H12 H 0.8116 0.6768 0.1641 0.0771 1.0000 Uiso . . . . . .
H21 H 0.5736 0.2217 0.0969 0.0530 1.0000 Uiso . . . . . .
H22 H 0.5711 0.4173 0.0854 0.0530 1.0000 Uiso . . . . . .
H31 H 0.6261 0.3286 0.5103 0.0585 1.0000 Uiso . . . . . .
H32 H 0.6079 0.5286 0.5610 0.0585 1.0000 Uiso . . . . . .
H41 H 0.4502 0.1340 0.2070 0.0614 1.0000 Uiso . . . . . .
H42 H 0.4125 0.2282 0.2474 0.0614 1.0000 Uiso . . . . . .
H51 H 0.6735 0.2970 0.2677 0.0609 1.0000 Uiso . . . . . .
H52 H 0.7501 0.2970 0.2839 0.0609 1.0000 Uiso . . . . . .
H61 H 0.8549 0.4609 0.4019 0.0578 1.0000 Uiso . . . . . .
H62 H 0.8824 0.4560 0.5720 0.0578 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2819(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.293(2) yes
Mn1 . O31 3_655 1.926(7) yes
Mn1 . O21 3_655 1.884(7) yes
Mn1 . O12 . 2.293(2) yes
Mn1 . O21 . 1.884(7) yes
Mn1 . O31 . 1.926(7) yes
Na1 . O11 3_655 2.316(9) yes
Na1 . O5 4_656 2.244(9) yes
Na1 . O11 2_546 2.414(9) yes
Na1 . O3 . 2.363(4) yes
Na1 . O5 . 2.288(10) yes
Na1 . O6 . 2.658(3) yes
Na2 . O12 3_655 2.628(9) yes
Na2 . O31 . 2.296(4) yes
Na2 . O41 . 2.328(6) yes
Na2 . O2 . 2.310(6) yes
Na2 . O3 . 2.281(3) yes
Na2 . O4 . 2.359(9) yes
Na3 . O4 3_656 2.325(8) yes
Na3 . O41 1_545 2.498(9) yes
Na3 . O41 3_646 2.498(9) yes
Na3 . O6 2_445 2.522(3) yes
Na3 . O6 4_646 2.522(3) yes
Na3 . O4 . 2.325(8) yes
C1 . O11 . 1.249(5) yes
C1 . O12 . 1.285(4) yes
C1 . C2 . 1.530(7) yes
C2 . O21 . 1.405(9) yes
C2 . C3 . 1.530(18) yes
C2 . H2 . 0.978 no
C3 . O31 . 1.427(8) yes
C3 . C4 . 1.543(7) yes
C3 . H3 . 1.011 no
C4 . O41 . 1.261(6) yes
C4 . O42 . 1.236(8) yes
O1 . H11 . 0.849 no
O1 . H12 . 0.809 no
O2 . H21 . 0.826 no
O2 . H22 . 0.854 no
O3 . H31 . 0.818 no
O3 . H32 . 0.846 no
O4 . H41 . 0.842 no
O4 . H42 . 0.847 no
O5 . H51 . 0.846 no
O5 . H52 . 0.840 no
O6 . H61 . 0.861 no
O6 . H62 . 0.876 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 87.5(2) yes
O12 3_655 Mn1 . O21 3_655 77.6(2) yes
O31 3_655 Mn1 . O21 3_655 85.4(2) yes
O12 3_655 Mn1 . O12 . 176.6(6) yes
O31 3_655 Mn1 . O12 . 94.8(2) yes
O21 3_655 Mn1 . O12 . 100.1(2) yes
O12 3_655 Mn1 . O21 . 100.1(2) yes
O31 3_655 Mn1 . O21 . 172.40(12) yes
O21 3_655 Mn1 . O21 . 95.8(5) yes
O12 . Mn1 . O21 . 77.6(2) yes
O12 3_655 Mn1 . O31 . 94.8(2) yes
O31 3_655 Mn1 . O31 . 94.4(4) yes
O21 3_655 Mn1 . O31 . 172.40(12) yes
O12 . Mn1 . O31 . 87.5(2) yes
O21 . Mn1 . O31 . 85.4(2) yes
O11 3_655 Na1 . O5 4_656 90.0(4) yes
O11 3_655 Na1 . O11 2_546 168.55(12) yes
O5 4_656 Na1 . O11 2_546 86.4(2) yes
O11 3_655 Na1 . O3 . 109.9(2) yes
O5 4_656 Na1 . O3 . 101.1(2) yes
O11 2_546 Na1 . O3 . 81.4(2) yes
O11 3_655 Na1 . O5 . 94.7(2) yes
O5 4_656 Na1 . O5 . 167.0(2) yes
O11 2_546 Na1 . O5 . 86.6(4) yes
O3 . Na1 . O5 . 88.7(2) yes
O11 3_655 Na1 . O6 . 84.7(2) yes
O5 4_656 Na1 . O6 . 88.17(19) yes
O11 2_546 Na1 . O6 . 84.3(2) yes
O3 . Na1 . O6 . 162.4(5) yes
O5 . Na1 . O6 . 80.2(2) yes
O12 3_655 Na2 . O31 . 78.2(2) yes
O12 3_655 Na2 . O41 . 93.0(3) yes
O31 . Na2 . O41 . 71.97(17) yes
O12 3_655 Na2 . O2 . 84.6(3) yes
O31 . Na2 . O2 . 83.86(19) yes
O41 . Na2 . O2 . 155.67(13) yes
O12 3_655 Na2 . O3 . 85.5(2) yes
O31 . Na2 . O3 . 163.2(3) yes
O41 . Na2 . O3 . 113.3(2) yes
O2 . Na2 . O3 . 90.74(17) yes
O12 3_655 Na2 . O4 . 171.01(16) yes
O31 . Na2 . O4 . 96.3(2) yes
O41 . Na2 . O4 . 92.0(2) yes
O2 . Na2 . O4 . 87.8(3) yes
O3 . Na2 . O4 . 99.4(3) yes
O4 3_656 Na3 . O41 1_545 161.79(19) yes
O4 3_656 Na3 . O41 3_646 87.5(2) yes
O41 1_545 Na3 . O41 3_646 86.1(4) yes
O4 3_656 Na3 . O6 2_445 87.8(2) yes
O41 1_545 Na3 . O6 2_445 79.0(2) yes
O41 3_646 Na3 . O6 2_445 112.8(2) yes
O4 3_656 Na3 . O6 4_646 82.6(2) yes
O41 1_545 Na3 . O6 4_646 112.8(2) yes
O41 3_646 Na3 . O6 4_646 79.0(2) yes
O6 2_445 Na3 . O6 4_646 164.5(6) yes
O4 3_656 Na3 . O4 . 103.4(5) yes
O41 1_545 Na3 . O4 . 87.5(2) yes
O41 3_646 Na3 . O4 . 161.79(19) yes
O6 2_445 Na3 . O4 . 82.6(2) yes
O6 4_646 Na3 . O4 . 87.8(2) yes
O11 . C1 . O12 . 124.2(5) yes
O11 . C1 . C2 . 119.7(3) yes
O12 . C1 . C2 . 116.1(3) yes
Na1 3_655 O11 . Na1 2_454 89.14(7) yes
Na1 3_655 O11 . C1 . 120.5(7) yes
Na1 2_454 O11 . C1 . 113.5(8) yes
Mn1 . O12 . C1 . 100.6(2) yes
Mn1 . O12 . Na2 3_655 83.4(2) yes
C1 . O12 . Na2 3_655 132.8(8) yes
C1 . C2 . O21 . 110.5(4) yes
C1 . C2 . C3 . 105.2(10) yes
O21 . C2 . C3 . 105.6(5) yes
C1 . C2 . H2 . 111.8 no
O21 . C2 . H2 . 113.9 no
C3 . C2 . H2 . 109.4 no
C2 . O21 . Mn1 . 102.5(7) yes
C2 . C3 . O31 . 106.9(5) yes
C2 . C3 . C4 . 108.2(10) yes
O31 . C3 . C4 . 112.8(4) yes
C2 . C3 . H3 . 110.6 no
O31 . C3 . H3 . 107.7 no
C4 . C3 . H3 . 110.6 no
Na2 . O31 . C3 . 116.3(2) yes
Na2 . O31 . Mn1 . 101.80(16) yes
C3 . O31 . Mn1 . 109.6(7) yes
C3 . C4 . O41 . 119.0(6) yes
C3 . C4 . O42 . 114.9(4) yes
O41 . C4 . O42 . 125.9(4) yes
Na2 . O41 . Na3 1_565 105.65(14) yes
Na2 . O41 . C4 . 118.2(5) yes
Na3 1_565 O41 . C4 . 117.4(9) yes
H11 . O1 . H12 . 87.1 no
Na2 . O2 . H21 . 144.1 no
Na2 . O2 . H22 . 95.2 no
H21 . O2 . H22 . 100.2 no
Na2 . O3 . Na1 . 113.85(19) yes
Na2 . O3 . H31 . 98.3 no
Na1 . O3 . H31 . 102.8 no
Na2 . O3 . H32 . 92.6 no
Na1 . O3 . H32 . 119.1 no
H31 . O3 . H32 . 127.4 no
Na3 . O4 . Na2 . 121.49(18) yes
Na3 . O4 . H41 . 112.1 no
Na2 . O4 . H41 . 106.6 no
Na3 . O4 . H42 . 121.0 no
Na2 . O4 . H42 . 103.9 no
H41 . O4 . H42 . 85.4 no
Na1 . O5 . Na1 4_646 94.22(8) yes
Na1 . O5 . H51 . 99.2 no
Na1 4_646 O5 . H51 . 123.7 no
Na1 . O5 . H52 . 106.1 no
Na1 4_646 O5 . H52 . 108.5 no
H51 . O5 . H52 . 119.2 no
Na3 2_555 O6 . Na1 . 173.9(4) yes
Na3 2_555 O6 . H61 . 87.3 no
Na1 . O6 . H61 . 92.8 no
Na3 2_555 O6 . H62 . 89.9 no
Na1 . O6 . H62 . 84.5 no
H61 . O6 . H62 . 117.2 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_10
_database_code_depnum_ccdc_archive 'CCDC 1419438'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_REFNR01_10                  
;
PROBLEM: Ratio of reflections to parameters is < 6
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT027_10                  
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_10                  
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_10                  
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_10                  
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_10                  
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_10                  
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_10                  
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.6368(15)
_cell_length_b                   6.512(2)
_cell_length_c                   9.5039(7)
_cell_angle_alpha                90
_cell_angle_beta                 113.862(4)
_cell_angle_gamma                90
_cell_volume                     1111.5(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.03 Fooo =    696.00 Mu =      8.08 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.03 FOOO =    696.00 Mu =      8.08 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.808

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.5536
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_ambient_pressure         3050
_diffrn_reflns_number            3036
_reflns_number_total             701
_diffrn_reflns_av_R_equivalents  0.038
# Number of reflections without Friedels Law is 701 
# Number of reflections with Friedels Law is 439 
# Theoretical number of reflections is about 790 


_diffrn_reflns_theta_min         1.602
_diffrn_reflns_theta_max         15.607
_diffrn_measured_fraction_theta_max 0.499

_diffrn_reflns_theta_full        11.705
_diffrn_measured_fraction_theta_full 0.515


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              -21
_reflns_limit_h_max              19
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              10

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.41
_refine_diff_density_max         0.45


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         693
_refine_ls_number_restraints     136
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0410
_refine_ls_wR_factor_ref         0.0604
_refine_ls_goodness_of_fit_ref   0.9978
_refine_ls_shift/su_max          0.0002137
_refine_ls_shift/su_mean         0.0000304


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        693
_refine_ls_R_factor_all          0.0410
_refine_ls_wR_factor_all         0.0604

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                645
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_gt          0.0597

_refine_ls_abs_structure_Flack   -0.07(8)
_refine_ls_abs_structure_details 'Flack (1983), 262 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8053(6) 0.0000 0.0260 1.0000 Uani S T . . . .
Na1 Na 0.73655(10) 0.5454(13) 0.4912(3) 0.0283 1.0000 Uani . . . . . .
Na2 Na 0.52166(9) 0.4973(10) 0.2886(2) 0.0311 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0262(13) 0.5000 0.0285 1.0000 Uani S T . . . .
C1 C 0.3503(2) 0.831(3) -0.2133(5) 0.0272 1.0000 Uani . U . . . .
O11 O 0.28536(14) 0.793(2) -0.3073(3) 0.0337 1.0000 Uani . U . . . .
O12 O 0.40811(15) 0.817(2) -0.2436(3) 0.0275 1.0000 Uani . U . . . .
C2 C 0.3644(2) 0.896(3) -0.0499(5) 0.0251 1.0000 Uani . U . . . .
O21 O 0.43361(16) 0.995(2) 0.0207(3) 0.0254 1.0000 Uani . U . . . .
C3 C 0.3733(2) 0.697(3) 0.0393(6) 0.0262 1.0000 Uani . U . . . .
O31 O 0.44075(16) 0.6044(19) 0.0492(4) 0.0266 1.0000 Uani . U . . . .
C4 C 0.3742(2) 0.749(3) 0.1989(5) 0.0301 1.0000 Uani . U . . . .
O41 O 0.43073(17) 0.7031(17) 0.3181(4) 0.0299 1.0000 Uani . U . . . .
O42 O 0.31625(19) 0.823(3) 0.1963(4) 0.0531 1.0000 Uani . U . . . .
O1 O 0.80900(17) 0.800(3) 0.1490(4) 0.0575 1.0000 Uani . . . . . .
O2 O 0.57702(14) 0.319(2) 0.1534(3) 0.0295 1.0000 Uani . U . . . .
O3 O 0.62452(18) 0.456(2) 0.5109(4) 0.0308 1.0000 Uani . U . . . .
O4 O 0.45815(16) 0.1947(18) 0.2913(4) 0.0309 1.0000 Uani . U . . . .
O5 O 0.71914(14) 0.280(2) 0.3230(3) 0.0332 1.0000 Uani . U . . . .
O6 O 0.87025(19) 0.525(2) 0.4868(4) 0.0290 1.0000 Uani . U . . . .
H2 H 0.3224 0.9815 -0.0474 0.0342 1.0000 Uiso . . . . . .
H3 H 0.3313 0.5965 -0.0161 0.0343 1.0000 Uiso . . . . . .
H11 H 0.7811 0.7998 0.1969 0.0867 1.0000 Uiso . . . . . .
H12 H 0.8115 0.6740 0.1630 0.0867 1.0000 Uiso . . . . . .
H21 H 0.5732 0.2165 0.0973 0.0500 1.0000 Uiso . . . . . .
H22 H 0.5710 0.4122 0.0880 0.0500 1.0000 Uiso . . . . . .
H31 H 0.6262 0.3237 0.5109 0.0519 1.0000 Uiso . . . . . .
H32 H 0.6081 0.5273 0.5612 0.0519 1.0000 Uiso . . . . . .
H41 H 0.4505 0.1352 0.2078 0.0530 1.0000 Uiso . . . . . .
H42 H 0.4126 0.2285 0.2478 0.0530 1.0000 Uiso . . . . . .
H51 H 0.6733 0.2921 0.2682 0.0543 1.0000 Uiso . . . . . .
H52 H 0.7500 0.2945 0.2830 0.0543 1.0000 Uiso . . . . . .
H61 H 0.8543 0.4618 0.4008 0.0472 1.0000 Uiso . . . . . .
H62 H 0.8820 0.4566 0.5713 0.0472 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2408(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.289(3) yes
Mn1 . O31 3_655 1.930(9) yes
Mn1 . O21 3_655 1.864(9) yes
Mn1 . O12 . 2.289(3) yes
Mn1 . O21 . 1.864(9) yes
Mn1 . O31 . 1.930(9) yes
Na1 . O11 3_655 2.287(13) yes
Na1 . O5 4_656 2.228(12) yes
Na1 . O11 2_546 2.409(12) yes
Na1 . O3 . 2.355(5) yes
Na1 . O5 . 2.285(13) yes
Na1 . O6 . 2.646(4) yes
Na2 . O12 3_655 2.624(12) yes
Na2 . O31 . 2.294(5) yes
Na2 . O41 . 2.339(8) yes
Na2 . O2 . 2.304(8) yes
Na2 . O3 . 2.272(4) yes
Na2 . O4 . 2.338(11) yes
Na3 . O4 3_656 2.315(10) yes
Na3 . O41 1_545 2.458(11) yes
Na3 . O41 3_646 2.458(11) yes
Na3 . O6 4_646 2.522(4) yes
Na3 . O6 2_445 2.522(4) yes
Na3 . O4 . 2.315(10) yes
C1 . O11 . 1.249(7) yes
C1 . O12 . 1.283(5) yes
C1 . C2 . 1.523(9) yes
C2 . O21 . 1.407(11) yes
C2 . C3 . 1.52(2) yes
C2 . H2 . 1.004 no
C3 . O31 . 1.422(11) yes
C3 . C4 . 1.547(9) yes
C3 . H3 . 1.017 no
C4 . O41 . 1.260(7) yes
C4 . O42 . 1.229(10) yes
O1 . H11 . 0.841 no
O1 . H12 . 0.827 no
O2 . H21 . 0.840 no
O2 . H22 . 0.841 no
O3 . H31 . 0.861 no
O3 . H32 . 0.821 no
O4 . H41 . 0.841 no
O4 . H42 . 0.848 no
O5 . H51 . 0.842 no
O5 . H52 . 0.840 no
O6 . H61 . 0.855 no
O6 . H62 . 0.865 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 87.7(3) yes
O12 3_655 Mn1 . O21 3_655 77.7(3) yes
O31 3_655 Mn1 . O21 3_655 84.7(3) yes
O12 3_655 Mn1 . O12 . 176.3(8) yes
O31 3_655 Mn1 . O12 . 94.7(3) yes
O21 3_655 Mn1 . O12 . 99.8(3) yes
O12 3_655 Mn1 . O21 . 99.8(3) yes
O31 3_655 Mn1 . O21 . 172.41(16) yes
O21 3_655 Mn1 . O21 . 96.9(6) yes
O12 . Mn1 . O21 . 77.7(3) yes
O12 3_655 Mn1 . O31 . 94.7(3) yes
O31 3_655 Mn1 . O31 . 94.6(6) yes
O21 3_655 Mn1 . O31 . 172.41(16) yes
O12 . Mn1 . O31 . 87.7(3) yes
O21 . Mn1 . O31 . 84.7(3) yes
O11 3_655 Na1 . O5 4_656 90.9(6) yes
O11 3_655 Na1 . O11 2_546 168.49(13) yes
O5 4_656 Na1 . O11 2_546 86.3(3) yes
O11 3_655 Na1 . O3 . 110.0(3) yes
O5 4_656 Na1 . O3 . 100.6(3) yes
O11 2_546 Na1 . O3 . 81.5(3) yes
O11 3_655 Na1 . O5 . 94.0(3) yes
O5 4_656 Na1 . O5 . 166.7(3) yes
O11 2_546 Na1 . O5 . 86.5(5) yes
O3 . Na1 . O5 . 89.3(3) yes
O11 3_655 Na1 . O6 . 84.5(3) yes
O5 4_656 Na1 . O6 . 88.6(2) yes
O11 2_546 Na1 . O6 . 84.3(3) yes
O3 . Na1 . O6 . 162.5(6) yes
O5 . Na1 . O6 . 79.6(3) yes
O12 3_655 Na2 . O31 . 78.2(3) yes
O12 3_655 Na2 . O41 . 92.4(3) yes
O31 . Na2 . O41 . 71.9(2) yes
O12 3_655 Na2 . O2 . 84.9(3) yes
O31 . Na2 . O2 . 83.9(2) yes
O41 . Na2 . O2 . 155.64(16) yes
O12 3_655 Na2 . O3 . 85.3(3) yes
O31 . Na2 . O3 . 163.1(4) yes
O41 . Na2 . O3 . 113.0(3) yes
O2 . Na2 . O3 . 90.9(2) yes
O12 3_655 Na2 . O4 . 171.0(2) yes
O31 . Na2 . O4 . 96.2(3) yes
O41 . Na2 . O4 . 92.6(3) yes
O2 . Na2 . O4 . 87.5(4) yes
O3 . Na2 . O4 . 99.6(4) yes
O4 3_656 Na3 . O41 1_545 162.1(2) yes
O4 3_656 Na3 . O41 3_646 86.5(3) yes
O41 1_545 Na3 . O41 3_646 88.4(5) yes
O4 3_656 Na3 . O6 4_646 82.7(3) yes
O41 1_545 Na3 . O6 4_646 113.0(3) yes
O41 3_646 Na3 . O6 4_646 78.5(3) yes
O4 3_656 Na3 . O6 2_445 87.8(3) yes
O41 1_545 Na3 . O6 2_445 78.5(3) yes
O41 3_646 Na3 . O6 2_445 113.0(3) yes
O6 4_646 Na3 . O6 2_445 164.7(8) yes
O4 3_656 Na3 . O4 . 103.2(6) yes
O41 1_545 Na3 . O4 . 86.5(3) yes
O41 3_646 Na3 . O4 . 162.1(2) yes
O6 4_646 Na3 . O4 . 87.8(3) yes
O6 2_445 Na3 . O4 . 82.7(3) yes
O11 . C1 . O12 . 124.4(6) yes
O11 . C1 . C2 . 119.7(4) yes
O12 . C1 . C2 . 115.9(4) yes
Na1 3_655 O11 . Na1 2_454 88.97(9) yes
Na1 3_655 O11 . C1 . 120.5(9) yes
Na1 2_454 O11 . C1 . 113.3(11) yes
Mn1 . O12 . C1 . 100.5(2) yes
Mn1 . O12 . Na2 3_655 83.6(3) yes
C1 . O12 . Na2 3_655 131.7(10) yes
C1 . C2 . O21 . 110.9(4) yes
C1 . C2 . C3 . 105.3(13) yes
O21 . C2 . C3 . 104.8(7) yes
C1 . C2 . H2 . 111.5 no
O21 . C2 . H2 . 112.1 no
C3 . C2 . H2 . 111.9 no
C2 . O21 . Mn1 . 103.1(9) yes
C2 . C3 . O31 . 107.0(7) yes
C2 . C3 . C4 . 108.3(14) yes
O31 . C3 . C4 . 112.7(5) yes
C2 . C3 . H3 . 111.9 no
O31 . C3 . H3 . 107.6 no
C4 . C3 . H3 . 109.4 no
Na2 . O31 . C3 . 116.6(3) yes
Na2 . O31 . Mn1 . 101.7(2) yes
C3 . O31 . Mn1 . 109.5(10) yes
C3 . C4 . O41 . 119.2(8) yes
C3 . C4 . O42 . 115.1(5) yes
O41 . C4 . O42 . 125.6(5) yes
Na2 . O41 . Na3 1_565 105.27(17) yes
Na2 . O41 . C4 . 117.7(6) yes
Na3 1_565 O41 . C4 . 120.0(11) yes
H11 . O1 . H12 . 85.6 no
Na2 . O2 . H21 . 144.5 no
Na2 . O2 . H22 . 95.3 no
H21 . O2 . H22 . 98.9 no
Na2 . O3 . Na1 . 113.8(2) yes
Na2 . O3 . H31 . 97.9 no
Na1 . O3 . H31 . 102.2 no
Na2 . O3 . H32 . 93.6 no
Na1 . O3 . H32 . 120.4 no
H31 . O3 . H32 . 126.1 no
Na3 . O4 . Na2 . 121.8(2) yes
Na3 . O4 . H41 . 112.8 no
Na2 . O4 . H41 . 105.7 no
Na3 . O4 . H42 . 121.2 no
Na2 . O4 . H42 . 103.7 no
H41 . O4 . H42 . 84.7 no
Na1 . O5 . Na1 4_646 93.67(10) yes
Na1 . O5 . H51 . 100.5 no
Na1 4_646 O5 . H51 . 122.1 no
Na1 . O5 . H52 . 107.5 no
Na1 4_646 O5 . H52 . 108.3 no
H51 . O5 . H52 . 119.7 no
Na3 2_555 O6 . Na1 . 174.1(6) yes
Na3 2_555 O6 . H61 . 87.5 no
Na1 . O6 . H61 . 93.2 no
Na3 2_555 O6 . H62 . 90.0 no
Na1 . O6 . H62 . 84.6 no
H61 . O6 . H62 . 119.7 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 1419439'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;

_vrf_PLAT027_11                  
;
PROBLEM: diffrn_reflns_theta_full (too) Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT029_11                  
;
PROBLEM: diffrn_measured_fraction_theta_full Low
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT090_11                  
;
PROBLEM: Poor Data/Parameter Ratio (Zmax > 18)
RESPONSE: The structure is non-centrosymmetric, and 
calculation of the data:parameter ratio 
assuming Friedel's law will give a value about 
50% of that expected for a centrosymmetric structure. Also exacerbated by shading of reciprocal space by the body of the pressure cell
;


_vrf_PLAT911_11                  
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT910_11                  
;
PROBLEM: Missing # FCF Refl Below Thmin
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT913_11                  
;
PROBLEM: Missing # of Very Strong Reflections in FCF
RESPONSE: Due to shading of reciprocal space by the body of the pressure cell
;

_vrf_PLAT341_11                  
;
PROBLEM: Low bond precision on C-C bonds
RESPONSE: Due to low completeness
;

_cell_length_a                   19.5753(19)
_cell_length_b                   6.476(3)
_cell_length_c                   9.5153(10)
_cell_angle_alpha                90
_cell_angle_beta                 114.033(6)
_cell_angle_gamma                90
_cell_volume                     1101.7(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.04 Fooo =    696.00 Mu =      8.15 M =    339.09
# Found Formula = C8 H28 Mn1 Na5 O24 
# Dc =      2.04 FOOO =    696.00 Mu =      8.15 M =    339.09

_chemical_formula_sum            'C8 H28 Mn1 Na5 O24'
_chemical_formula_moiety         'C8 H24 Mn Na5 O22, 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         678.17


_cell_measurement_reflns_used    0
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    293

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.815

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.4701
_exptl_absorpt_correction_T_max  0.7442
_diffrn_measurement_device_type  
'Rigaku CCD detector and Huber four-circle kappa goniometer'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  Silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_measurement_method       Omega

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Rigaku CrystalClear'
_computing_cell_refinement       'Bruker Apex2'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      293
_diffrn_reflns_number            3086
_reflns_number_total             921
_diffrn_reflns_av_R_equivalents  0.059
# Number of reflections without Friedels Law is 921 
# Number of reflections with Friedels Law is 595 
# Theoretical number of reflections is about 1128 


_diffrn_reflns_theta_min         1.602
_diffrn_reflns_theta_max         17.686
_diffrn_measured_fraction_theta_max 0.484

_diffrn_reflns_theta_full        15.917
_diffrn_measured_fraction_theta_full 0.491


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -24
_reflns_limit_h_max              22
_reflns_limit_k_min              -3
_reflns_limit_k_max              3
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.32
_refine_diff_density_max         1.43


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         911
_refine_ls_number_restraints     137
_refine_ls_number_parameters     174
_oxford_refine_ls_R_factor_ref   0.0774
_refine_ls_wR_factor_ref         0.0784
_refine_ls_goodness_of_fit_ref   0.9952
_refine_ls_shift/su_max          0.0001926
_refine_ls_shift/su_mean         0.0000361


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        911
_refine_ls_R_factor_all          0.0774
_refine_ls_wR_factor_all         0.0784

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                677
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_gt          0.0722

_refine_ls_abs_structure_Flack   0.06(10)
_refine_ls_abs_structure_details 'Flack (1983), 326 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mn1 Mn 0.5000 0.8039(8) 0.0000 0.0509 1.0000 Uani S T . . . .
Na1 Na 0.73623(14) 0.5426(17) 0.4914(3) 0.0522 1.0000 Uani . . . . . .
Na2 Na 0.52104(13) 0.5003(12) 0.2885(3) 0.0594 1.0000 Uani . . . . . .
Na3 Na 0.5000 -0.0251(17) 0.5000 0.0574 1.0000 Uani S T . . . .
C1 C 0.3498(3) 0.836(3) -0.2140(6) 0.0466 1.0000 Uani . U . . . .
O11 O 0.2858(2) 0.795(3) -0.3073(4) 0.0506 1.0000 Uani . U . . . .
O12 O 0.4084(2) 0.822(3) -0.2435(4) 0.0442 1.0000 Uani . U . . . .
C2 C 0.3639(3) 0.899(2) -0.0504(7) 0.0407 1.0000 Uani D U . . . .
O21 O 0.4340(2) 0.993(2) 0.0214(5) 0.0449 1.0000 Uani . U . . . .
C3 C 0.3714(3) 0.692(2) 0.0352(7) 0.0415 1.0000 Uani D U . . . .
O31 O 0.4408(2) 0.605(2) 0.0499(5) 0.0436 1.0000 Uani . U . . . .
C4 C 0.3726(3) 0.745(3) 0.1955(7) 0.0476 1.0000 Uani . U . . . .
O41 O 0.4304(2) 0.701(2) 0.3182(5) 0.0468 1.0000 Uani . U . . . .
O42 O 0.3142(2) 0.821(3) 0.1925(5) 0.0717 1.0000 Uani . U . . . .
O1 O 0.8097(2) 0.804(3) 0.1500(6) 0.0748 1.0000 Uani . . . . . .
O2 O 0.57707(18) 0.316(2) 0.1560(4) 0.0434 1.0000 Uani . U . . . .
O3 O 0.6250(2) 0.461(2) 0.5117(5) 0.0509 1.0000 Uani . U . . . .
O4 O 0.4583(2) 0.195(2) 0.2926(5) 0.0482 1.0000 Uani . U . . . .
O5 O 0.71824(19) 0.278(3) 0.3232(4) 0.0493 1.0000 Uani . U . . . .
O6 O 0.8701(2) 0.522(2) 0.4863(5) 0.0477 1.0000 Uani . U . . . .
H2 H 0.3227 0.9874 -0.0464 0.0488 1.0000 Uiso . . . . . .
H3 H 0.3288 0.5983 -0.0231 0.0502 1.0000 Uiso . . . . . .
H11 H 0.7813 0.8012 0.1967 0.1126 1.0000 Uiso . . . . . .
H12 H 0.8109 0.6750 0.1614 0.1126 1.0000 Uiso . . . . . .
H21 H 0.5736 0.2129 0.0994 0.0650 1.0000 Uiso . . . . . .
H22 H 0.5714 0.4080 0.0901 0.0650 1.0000 Uiso . . . . . .
H31 H 0.6265 0.3307 0.5124 0.0764 1.0000 Uiso . . . . . .
H32 H 0.6082 0.5334 0.5635 0.0764 1.0000 Uiso . . . . . .
H41 H 0.4508 0.1337 0.2098 0.0723 1.0000 Uiso . . . . . .
H42 H 0.4128 0.2284 0.2490 0.0723 1.0000 Uiso . . . . . .
H51 H 0.6722 0.2898 0.2686 0.0739 1.0000 Uiso . . . . . .
H52 H 0.7485 0.2910 0.2819 0.0739 1.0000 Uiso . . . . . .
H61 H 0.8537 0.4631 0.4002 0.0715 1.0000 Uiso . . . . . .
H62 H 0.8820 0.4599 0.5703 0.0715 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2154(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 . O12 3_655 2.283(4) yes
Mn1 . O31 3_655 1.918(11) yes
Mn1 . O21 3_655 1.849(11) yes
Mn1 . O12 . 2.283(4) yes
Mn1 . O21 . 1.849(11) yes
Mn1 . O31 . 1.918(11) yes
Na1 . O11 3_655 2.305(16) yes
Na1 . O11 2_546 2.381(16) yes
Na1 . O5 4_656 2.224(15) yes
Na1 . O3 . 2.324(6) yes
Na1 . O5 . 2.273(17) yes
Na1 . O6 . 2.643(5) yes
Na2 . O12 3_655 2.628(15) yes
Na2 . O31 . 2.276(7) yes
Na2 . O41 . 2.307(9) yes
Na2 . O2 . 2.313(10) yes
Na2 . O3 . 2.280(5) yes
Na2 . O4 . 2.334(13) yes
Na3 . O4 3_656 2.299(12) yes
Na3 . O41 1_545 2.464(13) yes
Na3 . O41 3_646 2.464(13) yes
Na3 . O6 2_445 2.511(4) yes
Na3 . O6 4_646 2.511(4) yes
Na3 . O4 . 2.299(12) yes
C1 . O11 . 1.233(9) yes
C1 . O12 . 1.290(7) yes
C1 . C2 . 1.523(10) yes
C2 . O21 . 1.398(11) yes
C2 . C3 . 1.545(9) yes
C2 . H2 . 1.001 no
C3 . O31 . 1.425(10) yes
C3 . C4 . 1.553(10) yes
C3 . H3 . 0.999 no
C4 . O41 . 1.284(8) yes
C4 . O42 . 1.233(12) yes
O1 . H11 . 0.841 no
O1 . H12 . 0.842 no
O2 . H21 . 0.842 no
O2 . H22 . 0.840 no
O3 . H31 . 0.841 no
O3 . H32 . 0.840 no
O4 . H41 . 0.842 no
O4 . H42 . 0.841 no
O5 . H51 . 0.841 no
O5 . H52 . 0.839 no
O6 . H61 . 0.840 no
O6 . H62 . 0.839 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O12 3_655 Mn1 . O31 3_655 88.9(3) yes
O12 3_655 Mn1 . O21 3_655 77.5(3) yes
O31 3_655 Mn1 . O21 3_655 84.1(3) yes
O12 3_655 Mn1 . O12 . 174.2(9) yes
O31 3_655 Mn1 . O12 . 95.0(3) yes
O21 3_655 Mn1 . O12 . 98.6(3) yes
O12 3_655 Mn1 . O21 . 98.6(3) yes
O31 3_655 Mn1 . O21 . 172.5(2) yes
O21 3_655 Mn1 . O21 . 97.2(8) yes
O12 . Mn1 . O21 . 77.5(3) yes
O12 3_655 Mn1 . O31 . 95.0(3) yes
O31 3_655 Mn1 . O31 . 95.5(7) yes
O21 3_655 Mn1 . O31 . 172.5(2) yes
O12 . Mn1 . O31 . 88.9(3) yes
O21 . Mn1 . O31 . 84.1(3) yes
O11 3_655 Na1 . O11 2_546 168.0(2) yes
O11 3_655 Na1 . O5 4_656 90.4(7) yes
O11 2_546 Na1 . O5 4_656 85.5(3) yes
O11 3_655 Na1 . O3 . 109.5(3) yes
O11 2_546 Na1 . O3 . 82.4(3) yes
O5 4_656 Na1 . O3 . 100.2(3) yes
O11 3_655 Na1 . O5 . 94.2(3) yes
O11 2_546 Na1 . O5 . 87.4(7) yes
O5 4_656 Na1 . O5 . 166.5(3) yes
O3 . Na1 . O5 . 90.3(4) yes
O11 3_655 Na1 . O6 . 84.4(3) yes
O11 2_546 Na1 . O6 . 84.2(3) yes
O5 4_656 Na1 . O6 . 88.2(3) yes
O3 . Na1 . O6 . 163.5(7) yes
O5 . Na1 . O6 . 79.6(3) yes
O12 3_655 Na2 . O31 . 78.3(4) yes
O12 3_655 Na2 . O41 . 93.1(4) yes
O31 . Na2 . O41 . 72.6(3) yes
O12 3_655 Na2 . O2 . 85.6(4) yes
O31 . Na2 . O2 . 84.1(3) yes
O41 . Na2 . O2 . 156.5(2) yes
O12 3_655 Na2 . O3 . 85.0(4) yes
O31 . Na2 . O3 . 162.7(5) yes
O41 . Na2 . O3 . 112.9(3) yes
O2 . Na2 . O3 . 90.4(3) yes
O12 3_655 Na2 . O4 . 171.1(3) yes
O31 . Na2 . O4 . 96.5(4) yes
O41 . Na2 . O4 . 92.2(3) yes
O2 . Na2 . O4 . 86.7(4) yes
O3 . Na2 . O4 . 99.5(4) yes
O4 3_656 Na3 . O41 1_545 162.0(3) yes
O4 3_656 Na3 . O41 3_646 86.7(3) yes
O41 1_545 Na3 . O41 3_646 88.0(6) yes
O4 3_656 Na3 . O6 2_445 88.1(3) yes
O41 1_545 Na3 . O6 2_445 78.0(3) yes
O41 3_646 Na3 . O6 2_445 112.5(4) yes
O4 3_656 Na3 . O6 4_646 83.2(3) yes
O41 1_545 Na3 . O6 4_646 112.5(4) yes
O41 3_646 Na3 . O6 4_646 78.0(3) yes
O6 2_445 Na3 . O6 4_646 166.0(9) yes
O4 3_656 Na3 . O4 . 103.2(7) yes
O41 1_545 Na3 . O4 . 86.7(3) yes
O41 3_646 Na3 . O4 . 162.0(3) yes
O6 2_445 Na3 . O4 . 83.2(3) yes
O6 4_646 Na3 . O4 . 88.1(3) yes
O11 . C1 . O12 . 124.0(7) yes
O11 . C1 . C2 . 120.1(5) yes
O12 . C1 . C2 . 115.8(5) yes
Na1 3_655 O11 . Na1 2_454 88.70(13) yes
Na1 3_655 O11 . C1 . 121.4(10) yes
Na1 2_454 O11 . C1 . 113.3(13) yes
Mn1 . O12 . C1 . 100.5(3) yes
Mn1 . O12 . Na2 3_655 83.0(4) yes
C1 . O12 . Na2 3_655 131.7(12) yes
C1 . C2 . O21 . 110.4(5) yes
C1 . C2 . C3 . 104.1(11) yes
O21 . C2 . C3 . 104.8(8) yes
C1 . C2 . H2 . 112.3 no
O21 . C2 . H2 . 112.4 no
C3 . C2 . H2 . 112.3 no
C2 . O21 . Mn1 . 104.5(10) yes
C2 . C3 . O31 . 106.2(8) yes
C2 . C3 . C4 . 106.7(11) yes
O31 . C3 . C4 . 111.0(5) yes
C2 . C3 . H3 . 111.0 no
O31 . C3 . H3 . 111.0 no
C4 . C3 . H3 . 110.7 no
Na2 . O31 . C3 . 117.3(4) yes
Na2 . O31 . Mn1 . 101.9(3) yes
C3 . O31 . Mn1 . 110.9(10) yes
C3 . C4 . O41 . 120.0(8) yes
C3 . C4 . O42 . 114.9(6) yes
O41 . C4 . O42 . 125.0(6) yes
Na2 . O41 . Na3 1_565 105.0(2) yes
Na2 . O41 . C4 . 116.8(6) yes
Na3 1_565 O41 . C4 . 120.7(12) yes
H11 . O1 . H12 . 84.2 no
Na2 . O2 . H21 . 145.6 no
Na2 . O2 . H22 . 95.2 no
H21 . O2 . H22 . 97.7 no
Na1 . O3 . Na2 . 114.1(3) yes
Na1 . O3 . H31 . 101.5 no
Na2 . O3 . H31 . 97.8 no
Na1 . O3 . H32 . 121.7 no
Na2 . O3 . H32 . 93.9 no
H31 . O3 . H32 . 125.2 no
Na3 . O4 . Na2 . 122.3(3) yes
Na3 . O4 . H41 . 112.0 no
Na2 . O4 . H41 . 106.1 no
Na3 . O4 . H42 . 121.1 no
Na2 . O4 . H42 . 103.6 no
H41 . O4 . H42 . 85.0 no
Na1 . O5 . Na1 4_646 93.49(14) yes
Na1 . O5 . H51 . 100.6 no
Na1 4_646 O5 . H51 . 122.4 no
Na1 . O5 . H52 . 108.4 no
Na1 4_646 O5 . H52 . 108.1 no
H51 . O5 . H52 . 119.1 no
Na3 2_555 O6 . Na1 . 174.5(6) yes
Na3 2_555 O6 . H61 . 88.4 no
Na1 . O6 . H61 . 93.1 no
Na3 2_555 O6 . H62 . 90.6 no
Na1 . O6 . H62 . 84.2 no
H61 . O6 . H62 . 124.0 no



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-11 -1 8 x .

