# 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_1H4
_database_code_depnum_ccdc_archive 'CCDC 1435095'
_audit_update_record             
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM74C
_cambridge_data_id               dw_k3_0007
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H62 N8 P4'
_chemical_formula_sum            'C30 H62 N8 P4'
_chemical_formula_weight         658.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.0734(9)
_cell_length_b                   12.3908(14)
_cell_length_c                   14.032(2)
_cell_angle_alpha                106.920(4)
_cell_angle_beta                 98.179(6)
_cell_angle_gamma                100.308(10)
_cell_volume                     972.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    29918
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      22.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_F_000             358
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.224
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4947
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.521
_diffrn_reflns_theta_max         22.442
_diffrn_reflns_theta_full        22.442
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             2396
_reflns_number_gt                2051
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          Twin

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+3.2317P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2396
_refine_ls_number_parameters     208
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0831
_refine_ls_wR_factor_ref         0.1937
_refine_ls_wR_factor_gt          0.1882
_refine_ls_goodness_of_fit_ref   1.282
_refine_ls_restrained_S_all      1.281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.075

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.5677(3) 0.43135(15) 0.23201(13) 0.0330(5) Uani 1 1 d . . . . .
P2 P 0.5654(3) 0.23113(15) 0.26259(13) 0.0343(5) Uani 1 1 d . . . . .
N1 N 0.3439(12) 0.1754(6) 0.3040(5) 0.0521(17) Uani 1 1 d D . . . .
H1 H 0.234(10) 0.212(6) 0.298(6) 0.07(3) Uiso 1 1 d D . . . .
N2 N 0.3532(10) 0.4936(5) 0.2555(5) 0.0393(14) Uani 1 1 d D . . . .
H2 H 0.224(6) 0.450(5) 0.258(5) 0.04(2) Uiso 1 1 d D . . . .
N3 N 0.4442(9) 0.2849(4) 0.1719(4) 0.0317(13) Uani 1 1 d . . . . .
N4 N 0.6343(10) 0.3772(4) 0.3310(4) 0.0358(14) Uani 1 1 d . . . . .
C1 C 0.2940(13) 0.0699(6) 0.3322(5) 0.0429(18) Uani 1 1 d . . . . .
C11 C 0.1075(18) -0.0229(8) 0.2509(6) 0.081(3) Uani 1 1 d . . . . .
H11A H 0.0637 -0.0892 0.2745 0.121 Uiso 1 1 calc R U . . .
H11B H 0.1646 -0.0483 0.1881 0.121 Uiso 1 1 calc R U . . .
H11C H -0.0260 0.0088 0.2377 0.121 Uiso 1 1 calc R U . . .
C12 C 0.2081(17) 0.1000(7) 0.4314(6) 0.068(3) Uani 1 1 d . . . . .
H12A H 0.1652 0.0296 0.4495 0.103 Uiso 1 1 calc R U . . .
H12B H 0.0744 0.1330 0.4227 0.103 Uiso 1 1 calc R U . . .
H12C H 0.3294 0.1567 0.4857 0.103 Uiso 1 1 calc R U . . .
C13 C 0.5076(15) 0.0257(8) 0.3480(8) 0.077(3) Uani 1 1 d . . . . .
H13A H 0.4748 -0.0409 0.3722 0.115 Uiso 1 1 calc R U . . .
H13B H 0.6282 0.0874 0.3986 0.115 Uiso 1 1 calc R U . . .
H13C H 0.5586 0.0019 0.2835 0.115 Uiso 1 1 calc R U . . .
C2 C 0.3265(12) 0.6073(6) 0.2510(5) 0.0365(16) Uani 1 1 d . . . . .
C21 C 0.1624(14) 0.5935(7) 0.1528(6) 0.058(2) Uani 1 1 d . . . . .
H21A H 0.1482 0.6701 0.1501 0.088 Uiso 1 1 calc R U . . .
H21B H 0.0119 0.5474 0.1511 0.088 Uiso 1 1 calc R U . . .
H21C H 0.2218 0.5539 0.0941 0.088 Uiso 1 1 calc R U . . .
C22 C 0.5573(13) 0.6840(6) 0.2556(6) 0.052(2) Uani 1 1 d . . . . .
H22A H 0.5367 0.7601 0.2539 0.079 Uiso 1 1 calc R U . . .
H22B H 0.6203 0.6475 0.1970 0.079 Uiso 1 1 calc R U . . .
H22C H 0.6630 0.6935 0.3187 0.079 Uiso 1 1 calc R U . . .
C23 C 0.2312(14) 0.6652(6) 0.3434(6) 0.051(2) Uani 1 1 d . . . . .
H23A H 0.2213 0.7436 0.3443 0.077 Uiso 1 1 calc R U . . .
H23B H 0.3328 0.6697 0.4060 0.077 Uiso 1 1 calc R U . . .
H23C H 0.0785 0.6194 0.3389 0.077 Uiso 1 1 calc R U . . .
C3 C 0.4145(12) 0.2272(6) 0.0600(5) 0.0370(17) Uani 1 1 d . . . . .
C31 C 0.2762(15) 0.1036(6) 0.0338(5) 0.053(2) Uani 1 1 d . . . . .
H31A H 0.2496 0.0644 -0.0397 0.080 Uiso 1 1 calc R U . . .
H31B H 0.1291 0.1048 0.0546 0.080 Uiso 1 1 calc R U . . .
H31C H 0.3608 0.0617 0.0698 0.080 Uiso 1 1 calc R U . . .
C32 C 0.6491(13) 0.2268(7) 0.0309(6) 0.051(2) Uani 1 1 d . . . . .
H32A H 0.6276 0.1857 -0.0421 0.077 Uiso 1 1 calc R U . . .
H32B H 0.7340 0.1876 0.0696 0.077 Uiso 1 1 calc R U . . .
H32C H 0.7353 0.3069 0.0466 0.077 Uiso 1 1 calc R U . . .
C33 C 0.2862(14) 0.2939(7) 0.0045(5) 0.052(2) Uani 1 1 d . . . . .
H33A H 0.2569 0.2543 -0.0691 0.077 Uiso 1 1 calc R U . . .
H33B H 0.3788 0.3728 0.0208 0.077 Uiso 1 1 calc R U . . .
H33C H 0.1405 0.2974 0.0262 0.077 Uiso 1 1 calc R U . . .
C4 C 0.8189(11) 0.4374(5) 0.4168(4) 0.0298(15) Uani 1 1 d . . . . .
C5 C 0.8116(12) 0.5444(6) 0.4815(5) 0.0356(17) Uani 1 1 d . . . . .
H5A H 0.6824 0.5758 0.4699 0.043 Uiso 1 1 calc R U . . .
C6 C 0.9922(12) 0.6064(6) 0.5633(5) 0.0362(17) Uani 1 1 d . . . . .
H6A H 0.9854 0.6803 0.6063 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N2 1.654(6) . ?
P1 N3 1.734(5) . ?
P1 N4 1.738(5) . ?
P1 P2 2.636(2) . ?
P2 N1 1.658(6) . ?
P2 N4 1.725(5) . ?
P2 N3 1.734(5) . ?
N1 C1 1.466(9) . ?
N1 H1 0.879(10) . ?
N2 C2 1.464(8) . ?
N2 H2 0.879(10) . ?
N3 C3 1.494(8) . ?
N4 C4 1.434(8) . ?
C1 C13 1.509(10) . ?
C1 C11 1.520(11) . ?
C1 C12 1.524(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C2 C21 1.528(10) . ?
C2 C22 1.528(10) . ?
C2 C23 1.533(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C3 C31 1.520(9) . ?
C3 C33 1.526(9) . ?
C3 C32 1.537(10) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C4 C6 1.381(9) 2_766 ?
C4 C5 1.385(9) . ?
C5 C6 1.392(9) . ?
C5 H5A 0.9500 . ?
C6 C4 1.381(9) 2_766 ?
C6 H6A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 P1 N3 105.7(3) . . ?
N2 P1 N4 106.3(3) . . ?
N3 P1 N4 79.5(2) . . ?
N2 P1 P2 118.9(2) . . ?
N1 P2 N4 104.8(3) . . ?
N1 P2 N3 103.9(3) . . ?
N4 P2 N3 79.9(2) . . ?
N1 P2 P1 116.8(2) . . ?
C1 N1 P2 130.9(5) . . ?
C1 N1 H1 118(6) . . ?
P2 N1 H1 111(5) . . ?
C2 N2 P1 128.4(5) . . ?
C2 N2 H2 112(5) . . ?
P1 N2 H2 118(5) . . ?
C3 N3 P2 123.3(4) . . ?
C3 N3 P1 122.9(4) . . ?
P2 N3 P1 98.9(3) . . ?
C4 N4 P2 127.0(4) . . ?
C4 N4 P1 122.8(4) . . ?
P2 N4 P1 99.1(3) . . ?
N1 C1 C13 110.3(6) . . ?
N1 C1 C11 110.6(6) . . ?
C13 C1 C11 110.3(7) . . ?
N1 C1 C12 108.2(6) . . ?
C13 C1 C12 109.1(7) . . ?
C11 C1 C12 108.3(7) . . ?
C1 C11 H11A 109.5 . . ?
C1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 C12 H12A 109.5 . . ?
C1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C13 H13A 109.5 . . ?
C1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C2 C21 110.2(6) . . ?
N2 C2 C22 110.6(6) . . ?
C21 C2 C22 109.2(6) . . ?
N2 C2 C23 108.1(5) . . ?
C21 C2 C23 110.0(6) . . ?
C22 C2 C23 108.8(6) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22A 109.5 . . ?
C2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 H23A 109.5 . . ?
C2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C3 C31 107.8(5) . . ?
N3 C3 C33 108.4(5) . . ?
C31 C3 C33 110.4(6) . . ?
N3 C3 C32 110.2(6) . . ?
C31 C3 C32 110.2(6) . . ?
C33 C3 C32 109.9(6) . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3 C32 H32A 109.5 . . ?
C3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C3 C33 H33A 109.5 . . ?
C3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C6 C4 C5 118.3(6) 2_766 . ?
C6 C4 N4 122.4(6) 2_766 . ?
C5 C4 N4 119.3(6) . . ?
C4 C5 C6 120.5(6) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C4 C6 C5 121.3(6) 2_766 . ?
C4 C6 H6A 119.4 2_766 . ?
C5 C6 H6A 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 P2 N1 C1 -135.5(7) . . . . ?
N3 P2 N1 C1 141.5(7) . . . . ?
P1 P2 N1 C1 -177.3(6) . . . . ?
N3 P1 N2 C2 -143.0(6) . . . . ?
N4 P1 N2 C2 133.6(6) . . . . ?
P2 P1 N2 C2 175.3(5) . . . . ?
N1 P2 N3 C3 -105.2(5) . . . . ?
N4 P2 N3 C3 151.9(5) . . . . ?
P1 P2 N3 C3 139.7(6) . . . . ?
N1 P2 N3 P1 115.2(3) . . . . ?
N4 P2 N3 P1 12.3(3) . . . . ?
N2 P1 N3 C3 103.7(5) . . . . ?
N4 P1 N3 C3 -152.1(5) . . . . ?
P2 P1 N3 C3 -139.9(6) . . . . ?
N2 P1 N3 P2 -116.4(3) . . . . ?
N4 P1 N3 P2 -12.2(3) . . . . ?
N1 P2 N4 C4 102.1(6) . . . . ?
N3 P2 N4 C4 -156.1(6) . . . . ?
P1 P2 N4 C4 -143.8(7) . . . . ?
N1 P2 N4 P1 -114.1(3) . . . . ?
N3 P2 N4 P1 -12.2(3) . . . . ?
N2 P1 N4 C4 -98.4(6) . . . . ?
N3 P1 N4 C4 158.1(5) . . . . ?
P2 P1 N4 C4 145.9(7) . . . . ?
N2 P1 N4 P2 115.7(3) . . . . ?
N3 P1 N4 P2 12.3(3) . . . . ?
P2 N1 C1 C13 16.1(11) . . . . ?
P2 N1 C1 C11 -106.3(9) . . . . ?
P2 N1 C1 C12 135.3(7) . . . . ?
P1 N2 C2 C21 101.9(7) . . . . ?
P1 N2 C2 C22 -18.9(9) . . . . ?
P1 N2 C2 C23 -137.9(6) . . . . ?
P2 N3 C3 C31 56.2(7) . . . . ?
P1 N3 C3 C31 -173.4(5) . . . . ?
P2 N3 C3 C33 175.7(5) . . . . ?
P1 N3 C3 C33 -53.9(7) . . . . ?
P2 N3 C3 C32 -64.0(7) . . . . ?
P1 N3 C3 C32 66.3(7) . . . . ?
P2 N4 C4 C6 20.9(9) . . . 2_766 ?
P1 N4 C4 C6 -115.3(6) . . . 2_766 ?
P2 N4 C4 C5 -160.5(5) . . . . ?
P1 N4 C4 C5 63.4(8) . . . . ?
C6 C4 C5 C6 0.9(11) 2_766 . . . ?
N4 C4 C5 C6 -177.8(6) . . . . ?
C4 C5 C6 C4 -0.9(11) . . . 2_766 ?


####################################################################### 
# 
# 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_1H4_cyclohexane
_database_code_depnum_ccdc_archive 'CCDC 1435096'
_audit_update_record             
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM74C
_cambridge_data_id               dw_b2_0013

_database_code_CSD               ?
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H62 N8 P4, 2(C6 H12)'
_chemical_formula_sum            'C42 H86 N8 P4'
_chemical_formula_weight         827.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.1188(3)
_cell_length_b                   14.0514(6)
_cell_length_c                   15.4022(7)
_cell_angle_alpha                88.944(3)
_cell_angle_beta                 89.034(3)
_cell_angle_gamma                81.094(2)
_cell_volume                     1307.93(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    5146
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      66.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_F_000             454
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.585
_shelx_estimated_absorpt_T_min   0.712
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14919
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.870
_diffrn_reflns_theta_max         66.648
_diffrn_reflns_theta_full        66.648
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             4576
_reflns_number_gt                2891
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1872P)²+0.9984P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4576
_refine_ls_number_parameters     237
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0985
_refine_ls_wR_factor_ref         0.3203
_refine_ls_wR_factor_gt          0.2805
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.084

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.7072(2) 0.66274(10) 0.79505(8) 0.0587(5) Uani 1 1 d . . . . .
P2 P 0.6053(2) 0.75270(10) 0.94129(9) 0.0579(4) Uani 1 1 d . . . . .
N1 N 0.5231(8) 0.5996(4) 0.7578(3) 0.0864(16) Uani 1 1 d . . . . .
H1A H 0.4048 0.6007 0.7901 0.104 Uiso 1 1 calc R U . . .
N2 N 0.3630(7) 0.7455(3) 0.9881(3) 0.0629(12) Uani 1 1 d . . . . .
H2A H 0.2749 0.7153 0.9590 0.076 Uiso 1 1 calc R U . . .
N3 N 0.5524(7) 0.7684(3) 0.8316(3) 0.0595(11) Uani 1 1 d . . . . .
N4 N 0.7100(7) 0.6385(3) 0.9051(3) 0.0600(11) Uani 1 1 d . . . . .
C1 C 0.5268(11) 0.5417(5) 0.6786(4) 0.0743(16) Uani 1 1 d . . . . .
C2 C 0.2768(9) 0.7835(4) 1.0726(3) 0.0637(14) Uani 1 1 d . . . . .
C3 C 0.5363(10) 0.8626(4) 0.7845(4) 0.0735(16) Uani 1 1 d . . . . .
C4 C 0.8547(8) 0.5678(3) 0.9522(3) 0.0530(11) Uani 1 1 d . . . . .
C5 C 0.7939(8) 0.5347(4) 1.0323(3) 0.0581(13) Uani 1 1 d . . . . .
H5A H 0.6521 0.5576 1.0548 0.070 Uiso 1 1 calc R U . . .
C6 C 1.0647(8) 0.5310(4) 0.9197(3) 0.0593(13) Uani 1 1 d . . . . .
H6A H 1.1099 0.5513 0.8646 0.071 Uiso 1 1 calc R U . . .
C11 C 0.3652(19) 0.5933(9) 0.6170(6) 0.168(5) Uani 1 1 d . . . . .
H11A H 0.3992 0.6576 0.6060 0.252 Uiso 1 1 calc R U . . .
H11B H 0.2173 0.5976 0.6418 0.252 Uiso 1 1 calc R U . . .
H11C H 0.3731 0.5585 0.5630 0.252 Uiso 1 1 calc R U . . .
C12 C 0.7492(14) 0.5267(9) 0.6383(6) 0.151(5) Uani 1 1 d . . . . .
H12A H 0.7979 0.5885 0.6282 0.226 Uiso 1 1 calc R U . . .
H12B H 0.7447 0.4943 0.5835 0.226 Uiso 1 1 calc R U . . .
H12C H 0.8517 0.4875 0.6768 0.226 Uiso 1 1 calc R U . . .
C13 C 0.4434(19) 0.4482(7) 0.7023(6) 0.149(4) Uani 1 1 d . . . . .
H13A H 0.2881 0.4618 0.7187 0.223 Uiso 1 1 calc R U . . .
H13B H 0.5274 0.4170 0.7506 0.223 Uiso 1 1 calc R U . . .
H13C H 0.4614 0.4060 0.6527 0.223 Uiso 1 1 calc R U . . .
C21 C 0.1271(12) 0.8784(5) 1.0597(5) 0.094(2) Uani 1 1 d . . . . .
H21A H 0.0130 0.8705 1.0186 0.142 Uiso 1 1 calc R U . . .
H21B H 0.2130 0.9262 1.0374 0.142 Uiso 1 1 calc R U . . .
H21C H 0.0588 0.8994 1.1148 0.142 Uiso 1 1 calc R U . . .
C22 C 0.1471(10) 0.7094(5) 1.1127(4) 0.0841(18) Uani 1 1 d . . . . .
H22A H 0.0264 0.7011 1.0750 0.126 Uiso 1 1 calc R U . . .
H22B H 0.0880 0.7314 1.1690 0.126 Uiso 1 1 calc R U . . .
H22C H 0.2442 0.6483 1.1198 0.126 Uiso 1 1 calc R U . . .
C23 C 0.4682(10) 0.7969(5) 1.1322(4) 0.0805(18) Uani 1 1 d . . . . .
H23A H 0.5445 0.8473 1.1085 0.121 Uiso 1 1 calc R U . . .
H23B H 0.5709 0.7371 1.1362 0.121 Uiso 1 1 calc R U . . .
H23C H 0.4101 0.8148 1.1896 0.121 Uiso 1 1 calc R U . . .
C31 C 0.7570(13) 0.8971(6) 0.7802(6) 0.116(3) Uani 1 1 d . . . . .
H31A H 0.8665 0.8475 0.7550 0.174 Uiso 1 1 calc R U . . .
H31B H 0.8011 0.9107 0.8383 0.174 Uiso 1 1 calc R U . . .
H31C H 0.7458 0.9552 0.7445 0.174 Uiso 1 1 calc R U . . .
C32 C 0.4469(15) 0.8506(5) 0.6942(5) 0.109(3) Uani 1 1 d . . . . .
H32A H 0.5363 0.7965 0.6662 0.163 Uiso 1 1 calc R U . . .
H32B H 0.4524 0.9088 0.6599 0.163 Uiso 1 1 calc R U . . .
H32C H 0.2950 0.8390 0.6992 0.163 Uiso 1 1 calc R U . . .
C33 C 0.3757(13) 0.9359(4) 0.8340(5) 0.092(2) Uani 1 1 d . . . . .
H33A H 0.2321 0.9148 0.8376 0.139 Uiso 1 1 calc R U . . .
H33B H 0.3619 0.9978 0.8040 0.139 Uiso 1 1 calc R U . . .
H33C H 0.4302 0.9420 0.8921 0.139 Uiso 1 1 calc R U . . .
C1S C 0.084(5) 0.1282(18) 0.6751(13) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H1S1 H -0.0343 0.1769 0.6974 0.267 Uiso 0.555(10) 1 calc R U P A 1
H1S2 H 0.1385 0.0818 0.7210 0.267 Uiso 0.555(10) 1 calc R U P A 1
C2S C 0.022(5) 0.0804(14) 0.5925(15) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H2S1 H -0.0699 0.0312 0.6078 0.267 Uiso 0.555(10) 1 calc R U P A 1
H2S2 H 0.1563 0.0488 0.5631 0.267 Uiso 0.555(10) 1 calc R U P A 1
C3S C -0.106(3) 0.1562(19) 0.5312(14) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H3S1 H -0.2229 0.1968 0.5635 0.267 Uiso 0.555(10) 1 calc R U P A 1
H3S2 H -0.1739 0.1243 0.4851 0.267 Uiso 0.555(10) 1 calc R U P A 1
C4S C 0.061(4) 0.219(2) 0.4908(16) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H4S1 H -0.0154 0.2708 0.4535 0.267 Uiso 0.555(10) 1 calc R U P A 1
H4S2 H 0.1770 0.1801 0.4569 0.267 Uiso 0.555(10) 1 calc R U P A 1
C5S C 0.163(4) 0.2635(16) 0.5761(17) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H5S1 H 0.2749 0.3034 0.5591 0.267 Uiso 0.555(10) 1 calc R U P A 1
H5S2 H 0.0463 0.3023 0.6102 0.267 Uiso 0.555(10) 1 calc R U P A 1
C6S C 0.269(3) 0.172(2) 0.6286(16) 0.222(4) Uiso 0.555(10) 1 d D U P A 1
H6S1 H 0.3500 0.1244 0.5890 0.267 Uiso 0.555(10) 1 calc R U P A 1
H6S2 H 0.3726 0.1890 0.6710 0.267 Uiso 0.555(10) 1 calc R U P A 1
C1T C 0.155(5) 0.205(3) 0.6630(16) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H1T1 H 0.2287 0.1545 0.7014 0.267 Uiso 0.445(10) 1 calc R U P A 2
H1T2 H 0.1352 0.2665 0.6940 0.267 Uiso 0.445(10) 1 calc R U P A 2
C2T C -0.073(5) 0.181(3) 0.6345(17) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H2T1 H -0.0732 0.1117 0.6390 0.267 Uiso 0.445(10) 1 calc R U P A 2
H2T2 H -0.1907 0.2136 0.6723 0.267 Uiso 0.445(10) 1 calc R U P A 2
C3T C -0.113(4) 0.216(2) 0.5401(19) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H3T1 H -0.0797 0.2818 0.5331 0.267 Uiso 0.445(10) 1 calc R U P A 2
H3T2 H -0.2685 0.2166 0.5258 0.267 Uiso 0.445(10) 1 calc R U P A 2
C4T C 0.037(5) 0.148(3) 0.4781(18) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H4T1 H 0.0486 0.1793 0.4212 0.267 Uiso 0.445(10) 1 calc R U P A 2
H4T2 H -0.0247 0.0884 0.4702 0.267 Uiso 0.445(10) 1 calc R U P A 2
C5T C 0.275(4) 0.125(2) 0.5223(19) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H5T1 H 0.2856 0.0665 0.5584 0.267 Uiso 0.445(10) 1 calc R U P A 2
H5T2 H 0.3924 0.1162 0.4779 0.267 Uiso 0.445(10) 1 calc R U P A 2
C6T C 0.295(5) 0.213(2) 0.578(2) 0.222(4) Uiso 0.445(10) 1 d D U P A 2
H6T1 H 0.2397 0.2728 0.5466 0.267 Uiso 0.445(10) 1 calc R U P A 2
H6T2 H 0.4500 0.2137 0.5927 0.267 Uiso 0.445(10) 1 calc R U P A 2


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.654(5) . ?
P1 N4 1.722(4) . ?
P1 N3 1.731(4) . ?
P1 P2 2.6218(19) . ?
P2 N2 1.654(4) . ?
P2 N3 1.729(4) . ?
P2 N4 1.731(4) . ?
N1 C1 1.477(7) . ?
N1 H1A 0.8700 . ?
N2 C2 1.474(7) . ?
N2 H2A 0.8700 . ?
N3 C3 1.489(7) . ?
N4 C4 1.422(6) . ?
C1 C12 1.473(10) . ?
C1 C11 1.479(10) . ?
C1 C13 1.517(11) . ?
C2 C21 1.508(8) . ?
C2 C22 1.521(9) . ?
C2 C23 1.536(7) . ?
C3 C31 1.503(9) . ?
C3 C33 1.516(9) . ?
C3 C32 1.525(9) . ?
C4 C5 1.376(7) . ?
C4 C6 1.397(7) . ?
C5 C6 1.378(7) 2_767 ?
C5 H5A 0.9400 . ?
C6 C5 1.378(7) 2_767 ?
C6 H6A 0.9400 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N4 104.0(3) . . ?
N1 P1 N3 104.8(2) . . ?
N4 P1 N3 80.3(2) . . ?
N1 P1 P2 116.48(18) . . ?
N2 P2 N3 105.4(2) . . ?
N2 P2 N4 106.8(2) . . ?
N3 P2 N4 80.1(2) . . ?
N2 P2 P1 118.77(16) . . ?
C1 N1 P1 130.5(4) . . ?
C1 N1 H1A 114.7 . . ?
P1 N1 H1A 114.7 . . ?
C2 N2 P2 128.5(4) . . ?
C2 N2 H2A 115.8 . . ?
P2 N2 H2A 115.8 . . ?
C3 N3 P2 124.1(4) . . ?
C3 N3 P1 123.9(4) . . ?
P2 N3 P1 98.6(2) . . ?
C4 N4 P1 128.5(3) . . ?
C4 N4 P2 125.4(3) . . ?
P1 N4 P2 98.8(2) . . ?
C12 C1 N1 110.8(5) . . ?
C12 C1 C11 109.9(8) . . ?
N1 C1 C11 108.4(6) . . ?
C12 C1 C13 113.1(8) . . ?
N1 C1 C13 108.4(6) . . ?
C11 C1 C13 106.0(8) . . ?
N2 C2 C21 110.1(5) . . ?
N2 C2 C22 106.7(5) . . ?
C21 C2 C22 110.1(5) . . ?
N2 C2 C23 110.4(4) . . ?
C21 C2 C23 109.8(5) . . ?
C22 C2 C23 109.7(5) . . ?
N3 C3 C31 111.0(5) . . ?
N3 C3 C33 108.2(5) . . ?
C31 C3 C33 108.3(6) . . ?
N3 C3 C32 108.1(5) . . ?
C31 C3 C32 111.7(6) . . ?
C33 C3 C32 109.5(5) . . ?
C5 C4 C6 117.8(4) . . ?
C5 C4 N4 121.0(4) . . ?
C6 C4 N4 121.2(4) . . ?
C4 C5 C6 121.7(4) . 2_767 ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 2_767 . ?
C5 C6 C4 120.4(5) 2_767 . ?
C5 C6 H6A 119.8 2_767 . ?
C4 C6 H6A 119.8 . . ?
C1 C11 H11A 109.5 . . ?
C1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 C12 H12A 109.5 . . ?
C1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C13 H13A 109.5 . . ?
C1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22A 109.5 . . ?
C2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 H23A 109.5 . . ?
C2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3 C32 H32A 109.5 . . ?
C3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C3 C33 H33A 109.5 . . ?
C3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 P1 N1 C1 -138.8(6) . . . . ?
N3 P1 N1 C1 137.8(6) . . . . ?
P2 P1 N1 C1 179.7(5) . . . . ?
N3 P2 N2 C2 -143.0(5) . . . . ?
N4 P2 N2 C2 132.9(5) . . . . ?
P1 P2 N2 C2 175.1(4) . . . . ?
N2 P2 N3 C3 102.0(4) . . . . ?
N4 P2 N3 C3 -153.1(5) . . . . ?
P1 P2 N3 C3 -141.6(5) . . . . ?
N2 P2 N3 P1 -116.4(2) . . . . ?
N4 P2 N3 P1 -11.5(2) . . . . ?
N1 P1 N3 C3 -104.7(5) . . . . ?
N4 P1 N3 C3 153.2(5) . . . . ?
P2 P1 N3 C3 141.6(5) . . . . ?
N1 P1 N3 P2 113.6(3) . . . . ?
N4 P1 N3 P2 11.6(2) . . . . ?
N1 P1 N4 C4 94.8(5) . . . . ?
N3 P1 N4 C4 -162.3(5) . . . . ?
P2 P1 N4 C4 -150.7(6) . . . . ?
N1 P1 N4 P2 -114.5(3) . . . . ?
N3 P1 N4 P2 -11.6(2) . . . . ?
N2 P2 N4 C4 -93.2(4) . . . . ?
N3 P2 N4 C4 163.6(5) . . . . ?
P1 P2 N4 C4 152.0(5) . . . . ?
N2 P2 N4 P1 114.8(2) . . . . ?
N3 P2 N4 P1 11.6(2) . . . . ?
P1 N1 C1 C12 12.2(10) . . . . ?
P1 N1 C1 C11 -108.4(8) . . . . ?
P1 N1 C1 C13 136.9(7) . . . . ?
P2 N2 C2 C21 98.4(6) . . . . ?
P2 N2 C2 C22 -142.2(5) . . . . ?
P2 N2 C2 C23 -23.1(7) . . . . ?
P2 N3 C3 C31 67.5(7) . . . . ?
P1 N3 C3 C31 -64.7(7) . . . . ?
P2 N3 C3 C33 -51.2(6) . . . . ?
P1 N3 C3 C33 176.6(4) . . . . ?
P2 N3 C3 C32 -169.7(5) . . . . ?
P1 N3 C3 C32 58.1(6) . . . . ?
P1 N4 C4 C5 -157.5(4) . . . . ?
P2 N4 C4 C5 58.9(6) . . . . ?
P1 N4 C4 C6 23.9(7) . . . . ?
P2 N4 C4 C6 -119.8(5) . . . . ?
C6 C4 C5 C6 1.3(9) . . . 2_767 ?
N4 C4 C5 C6 -177.4(5) . . . 2_767 ?
C5 C4 C6 C5 -1.3(9) . . . 2_767 ?
N4 C4 C6 C5 177.4(5) . . . 2_767 ?


####################################################################### 
# 
# 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_1H4_cyclohexane_SQUEEZED
_database_code_depnum_ccdc_archive 'CCDC 1435097'
_audit_update_record             
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM74C
_cambridge_data_id               dw_b2_0013
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H62 N8 P4'
_chemical_formula_sum            'C30 H62 N8 P4'
_chemical_formula_weight         658.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.1188(3)
_cell_length_b                   14.0514(6)
_cell_length_c                   15.4022(7)
_cell_angle_alpha                88.944(3)
_cell_angle_beta                 89.034(3)
_cell_angle_gamma                81.094(3)
_cell_volume                     1307.93(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    5146
_cell_measurement_theta_min      4.25
_cell_measurement_theta_max      66.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.836
_exptl_crystal_F_000             358
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.502
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14904
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.870
_diffrn_reflns_theta_max         66.648
_diffrn_reflns_theta_full        66.648
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             4573
_reflns_number_gt                2888
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

Structure factors included contributions from the .fab file.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1059P)²+0.7013P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4573
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2135
_refine_ls_wR_factor_gt          0.1880
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.059

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.70718(16) 0.66270(7) 0.79505(6) 0.0580(3) Uani 1 1 d . . . . .
P2 P 0.60531(15) 0.75264(7) 0.94130(7) 0.0569(3) Uani 1 1 d . . . . .
N1 N 0.5230(6) 0.6000(3) 0.7573(2) 0.0838(11) Uani 1 1 d . . . . .
H1A H 0.4039 0.6018 0.7893 0.101 Uiso 1 1 calc R U . . .
N2 N 0.3638(5) 0.7458(2) 0.9881(2) 0.0610(8) Uani 1 1 d . . . . .
H2A H 0.2750 0.7163 0.9587 0.073 Uiso 1 1 calc R U . . .
N3 N 0.5523(5) 0.7680(2) 0.8319(2) 0.0574(8) Uani 1 1 d . . . . .
N4 N 0.7097(5) 0.6385(2) 0.90530(19) 0.0586(8) Uani 1 1 d . . . . .
C1 C 0.5261(8) 0.5417(3) 0.6790(3) 0.0727(12) Uani 1 1 d . . . . .
C2 C 0.2778(6) 0.7829(3) 1.0728(3) 0.0631(10) Uani 1 1 d . . . . .
C3 C 0.5358(7) 0.8622(3) 0.7848(3) 0.0727(11) Uani 1 1 d . . . . .
C4 C 0.8550(6) 0.5682(2) 0.9519(2) 0.0504(8) Uani 1 1 d . . . . .
C5 C 0.7947(6) 0.5352(3) 1.0322(2) 0.0574(9) Uani 1 1 d . . . . .
H5A H 0.6534 0.5584 1.0550 0.069 Uiso 1 1 calc R U . . .
C6 C 1.0637(6) 0.5311(3) 0.9196(2) 0.0582(9) Uani 1 1 d . . . . .
H6A H 1.1091 0.5512 0.8646 0.070 Uiso 1 1 calc R U . . .
C11 C 0.3641(13) 0.5932(6) 0.6172(5) 0.165(3) Uani 1 1 d . . . . .
H11A H 0.2257 0.6148 0.6476 0.247 Uiso 1 1 calc R U . . .
H11B H 0.3390 0.5500 0.5713 0.247 Uiso 1 1 calc R U . . .
H11C H 0.4216 0.6483 0.5923 0.247 Uiso 1 1 calc R U . . .
C12 C 0.7514(10) 0.5256(6) 0.6392(5) 0.165(4) Uani 1 1 d . . . . .
H12A H 0.8047 0.5868 0.6318 0.248 Uiso 1 1 calc R U . . .
H12B H 0.7461 0.4959 0.5831 0.248 Uiso 1 1 calc R U . . .
H12C H 0.8506 0.4835 0.6768 0.248 Uiso 1 1 calc R U . . .
C13 C 0.4387(13) 0.4497(5) 0.7008(4) 0.143(3) Uani 1 1 d . . . . .
H13A H 0.2961 0.4646 0.7300 0.214 Uiso 1 1 calc R U . . .
H13B H 0.5414 0.4098 0.7387 0.214 Uiso 1 1 calc R U . . .
H13C H 0.4221 0.4154 0.6479 0.214 Uiso 1 1 calc R U . . .
C21 C 0.1259(8) 0.8788(4) 1.0595(3) 0.0947(16) Uani 1 1 d . . . . .
H21A H 0.0071 0.8700 1.0210 0.142 Uiso 1 1 calc R U . . .
H21B H 0.2101 0.9256 1.0341 0.142 Uiso 1 1 calc R U . . .
H21C H 0.0640 0.9017 1.1151 0.142 Uiso 1 1 calc R U . . .
C22 C 0.1471(8) 0.7101(4) 1.1124(3) 0.0835(13) Uani 1 1 d . . . . .
H22A H 0.0214 0.7050 1.0762 0.125 Uiso 1 1 calc R U . . .
H22B H 0.0950 0.7305 1.1699 0.125 Uiso 1 1 calc R U . . .
H22C H 0.2407 0.6478 1.1166 0.125 Uiso 1 1 calc R U . . .
C23 C 0.4674(7) 0.7971(4) 1.1317(3) 0.0805(13) Uani 1 1 d . . . . .
H23A H 0.5481 0.8450 1.1059 0.121 Uiso 1 1 calc R U . . .
H23B H 0.5663 0.7366 1.1387 0.121 Uiso 1 1 calc R U . . .
H23C H 0.4083 0.8189 1.1880 0.121 Uiso 1 1 calc R U . . .
C31 C 0.7608(9) 0.8962(4) 0.7793(4) 0.115(2) Uani 1 1 d . . . . .
H31A H 0.8675 0.8472 0.7519 0.173 Uiso 1 1 calc R U . . .
H31B H 0.8093 0.9076 0.8373 0.173 Uiso 1 1 calc R U . . .
H31C H 0.7486 0.9555 0.7452 0.173 Uiso 1 1 calc R U . . .
C32 C 0.4443(10) 0.8505(4) 0.6951(3) 0.1071(18) Uani 1 1 d . . . . .
H32A H 0.5438 0.8022 0.6637 0.161 Uiso 1 1 calc R U . . .
H32B H 0.4307 0.9115 0.6636 0.161 Uiso 1 1 calc R U . . .
H32C H 0.3000 0.8305 0.7009 0.161 Uiso 1 1 calc R U . . .
C33 C 0.3755(9) 0.9365(3) 0.8353(3) 0.0946(16) Uani 1 1 d . . . . .
H33A H 0.2354 0.9131 0.8436 0.142 Uiso 1 1 calc R U . . .
H33B H 0.3521 0.9969 0.8028 0.142 Uiso 1 1 calc R U . . .
H33C H 0.4374 0.9464 0.8913 0.142 Uiso 1 1 calc R U . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 N1 1.653(4) . ?
P1 N4 1.725(3) . ?
P1 N3 1.729(3) . ?
P1 P2 2.6217(14) . ?
P2 N2 1.648(3) . ?
P2 N3 1.724(3) . ?
P2 N4 1.729(3) . ?
N1 C1 1.468(5) . ?
N1 H1A 0.8700 . ?
N2 C2 1.472(5) . ?
N2 H2A 0.8700 . ?
N3 C3 1.488(5) . ?
N4 C4 1.416(4) . ?
C1 C12 1.486(7) . ?
C1 C11 1.482(7) . ?
C1 C13 1.504(7) . ?
C2 C22 1.507(6) . ?
C2 C23 1.525(5) . ?
C2 C21 1.526(6) . ?
C3 C32 1.520(6) . ?
C3 C31 1.526(6) . ?
C3 C33 1.531(6) . ?
C4 C5 1.378(5) . ?
C4 C6 1.390(5) . ?
C5 C6 1.384(5) 2_767 ?
C5 H5A 0.9400 . ?
C6 C5 1.384(5) 2_767 ?
C6 H6A 0.9400 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N4 104.28(18) . . ?
N1 P1 N3 104.63(17) . . ?
N4 P1 N3 80.04(15) . . ?
N1 P1 P2 116.63(13) . . ?
N2 P2 N3 105.42(15) . . ?
N2 P2 N4 106.94(16) . . ?
N3 P2 N4 80.05(15) . . ?
N2 P2 P1 118.95(12) . . ?
C1 N1 P1 131.0(3) . . ?
C1 N1 H1A 114.5 . . ?
P1 N1 H1A 114.5 . . ?
C2 N2 P2 128.9(3) . . ?
C2 N2 H2A 115.6 . . ?
P2 N2 H2A 115.6 . . ?
C3 N3 P2 124.0(3) . . ?
C3 N3 P1 123.8(3) . . ?
P2 N3 P1 98.79(15) . . ?
C4 N4 P1 128.1(2) . . ?
C4 N4 P2 125.6(2) . . ?
P1 N4 P2 98.73(16) . . ?
N1 C1 C12 110.5(4) . . ?
N1 C1 C11 108.3(5) . . ?
C12 C1 C11 110.6(6) . . ?
N1 C1 C13 109.6(4) . . ?
C12 C1 C13 113.2(6) . . ?
C11 C1 C13 104.4(5) . . ?
N2 C2 C22 107.4(3) . . ?
N2 C2 C23 110.5(3) . . ?
C22 C2 C23 110.4(4) . . ?
N2 C2 C21 109.5(3) . . ?
C22 C2 C21 109.5(4) . . ?
C23 C2 C21 109.5(4) . . ?
N3 C3 C32 108.2(4) . . ?
N3 C3 C31 110.7(4) . . ?
C32 C3 C31 111.6(4) . . ?
N3 C3 C33 108.3(3) . . ?
C32 C3 C33 109.4(4) . . ?
C31 C3 C33 108.6(4) . . ?
C5 C4 C6 117.5(3) . . ?
C5 C4 N4 120.7(3) . . ?
C6 C4 N4 121.8(3) . . ?
C4 C5 C6 121.9(3) . 2_767 ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 2_767 . ?
C5 C6 C4 120.6(3) 2_767 . ?
C5 C6 H6A 119.7 2_767 . ?
C4 C6 H6A 119.7 . . ?
C1 C11 H11A 109.5 . . ?
C1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 C12 H12A 109.5 . . ?
C1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C13 H13A 109.5 . . ?
C1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22A 109.5 . . ?
C2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 H23A 109.5 . . ?
C2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3 C32 H32A 109.5 . . ?
C3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C3 C33 H33A 109.5 . . ?
C3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 P1 N1 C1 -138.2(4) . . . . ?
N3 P1 N1 C1 138.6(4) . . . . ?
P2 P1 N1 C1 -179.8(4) . . . . ?
N3 P2 N2 C2 -143.8(3) . . . . ?
N4 P2 N2 C2 132.1(3) . . . . ?
P1 P2 N2 C2 174.5(3) . . . . ?
N2 P2 N3 C3 101.8(3) . . . . ?
N4 P2 N3 C3 -153.2(3) . . . . ?
P1 P2 N3 C3 -141.5(4) . . . . ?
N2 P2 N3 P1 -116.70(16) . . . . ?
N4 P2 N3 P1 -11.72(15) . . . . ?
N1 P1 N3 C3 -104.3(3) . . . . ?
N4 P1 N3 C3 153.4(3) . . . . ?
P2 P1 N3 C3 141.6(4) . . . . ?
N1 P1 N3 P2 114.04(19) . . . . ?
N4 P1 N3 P2 11.75(15) . . . . ?
N1 P1 N4 C4 95.3(3) . . . . ?
N3 P1 N4 C4 -162.0(3) . . . . ?
P2 P1 N4 C4 -150.3(4) . . . . ?
N1 P1 N4 P2 -114.42(19) . . . . ?
N3 P1 N4 P2 -11.71(15) . . . . ?
N2 P2 N4 C4 -93.6(3) . . . . ?
N3 P2 N4 C4 163.1(3) . . . . ?
P1 P2 N4 C4 151.4(4) . . . . ?
N2 P2 N4 P1 114.97(17) . . . . ?
N3 P2 N4 P1 11.74(15) . . . . ?
P1 N1 C1 C12 12.2(7) . . . . ?
P1 N1 C1 C11 -109.1(6) . . . . ?
P1 N1 C1 C13 137.6(5) . . . . ?
P2 N2 C2 C22 -142.3(3) . . . . ?
P2 N2 C2 C23 -21.8(5) . . . . ?
P2 N2 C2 C21 98.9(4) . . . . ?
P2 N3 C3 C32 -169.1(3) . . . . ?
P1 N3 C3 C32 58.7(5) . . . . ?
P2 N3 C3 C31 68.3(5) . . . . ?
P1 N3 C3 C31 -63.9(5) . . . . ?
P2 N3 C3 C33 -50.6(5) . . . . ?
P1 N3 C3 C33 177.2(3) . . . . ?
P1 N4 C4 C5 -157.9(3) . . . . ?
P2 N4 C4 C5 59.1(5) . . . . ?
P1 N4 C4 C6 23.3(5) . . . . ?
P2 N4 C4 C6 -119.7(4) . . . . ?
C6 C4 C5 C6 1.1(6) . . . 2_767 ?
N4 C4 C5 C6 -177.8(3) . . . 2_767 ?
C5 C4 C6 C5 -1.1(6) . . . 2_767 ?
N4 C4 C6 C5 177.8(3) . . . 2_767 ?



####################################################################### 
# 
# 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_1Mg2
_database_code_depnum_ccdc_archive 'CCDC 1435098'
_audit_update_record             
;
2015-11-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2014/7

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.0  (Andrew D. Bond, July 2015)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Raquel Sevilla-Martin'
_cambridge_user_crsid            rs617
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RSM86
_cambridge_data_id               dw_k3_0016
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H90 Mg2 N8 O4 P4'
_chemical_formula_sum            'C46 H90 Mg2 N8 O4 P4'
_chemical_formula_weight         991.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4939(4)
_cell_length_b                   17.4459(6)
_cell_length_c                   16.1229(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.9488(16)
_cell_angle_gamma                90
_cell_volume                     2930.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    33709
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_F_000             1076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.194
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17185
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.588
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             5034
_reflns_number_gt                3667
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+4.0095P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5034
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1431
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.056

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.36142(11) 0.29014(7) 0.26343(7) 0.0414(3) Uani 1 1 d . . . . .
P1 P 0.50166(9) 0.27162(5) 0.42318(5) 0.0370(2) Uani 1 1 d . . . . .
P2 P 0.60362(9) 0.35992(5) 0.30933(6) 0.0400(3) Uani 1 1 d . . . . .
N1 N 0.3509(3) 0.25641(17) 0.38499(18) 0.0409(7) Uani 1 1 d . . . . .
C1 C 0.2654(4) 0.2133(2) 0.4352(2) 0.0494(10) Uani 1 1 d . . . . .
C11 C 0.3116(5) 0.1303(2) 0.4493(3) 0.0671(13) Uani 1 1 d . . . . .
H11A H 0.3967 0.1301 0.4818 0.101 Uiso 1 1 calc R U . . .
H11B H 0.3165 0.1055 0.3952 0.101 Uiso 1 1 calc R U . . .
H11C H 0.2511 0.1022 0.4798 0.101 Uiso 1 1 calc R U . . .
C12 C 0.2555(5) 0.2499(3) 0.5203(3) 0.0678(13) Uani 1 1 d . . . . .
H12A H 0.2200 0.3017 0.5123 0.102 Uiso 1 1 calc R U . . .
H12B H 0.3411 0.2527 0.5521 0.102 Uiso 1 1 calc R U . . .
H12C H 0.1992 0.2188 0.5510 0.102 Uiso 1 1 calc R U . . .
C13 C 0.1314(4) 0.2116(3) 0.3870(3) 0.0750(14) Uani 1 1 d . . . . .
H13A H 0.0972 0.2639 0.3815 0.113 Uiso 1 1 calc R U . . .
H13B H 0.0751 0.1799 0.4171 0.113 Uiso 1 1 calc R U . . .
H13C H 0.1357 0.1899 0.3313 0.113 Uiso 1 1 calc R U . . .
N2 N 0.4866(3) 0.37369(16) 0.23303(18) 0.0438(7) Uani 1 1 d . . . . .
C2 C 0.4909(4) 0.4381(2) 0.1740(2) 0.0493(10) Uani 1 1 d . . . . .
C21 C 0.4704(7) 0.5135(3) 0.2137(4) 0.106(2) Uani 1 1 d . . . . .
H21A H 0.3871 0.5133 0.2355 0.159 Uiso 1 1 calc R U . . .
H21B H 0.4715 0.5543 0.1721 0.159 Uiso 1 1 calc R U . . .
H21C H 0.5388 0.5224 0.2596 0.159 Uiso 1 1 calc R U . . .
C22 C 0.6201(8) 0.4435(5) 0.1413(5) 0.170(4) Uani 1 1 d . . . . .
H22A H 0.6882 0.4469 0.1885 0.255 Uiso 1 1 calc R U . . .
H22B H 0.6220 0.4893 0.1063 0.255 Uiso 1 1 calc R U . . .
H22C H 0.6335 0.3978 0.1081 0.255 Uiso 1 1 calc R U . . .
C23 C 0.3886(10) 0.4276(4) 0.1024(4) 0.181(5) Uani 1 1 d . . . . .
H23A H 0.3067 0.4170 0.1236 0.272 Uiso 1 1 calc R U . . .
H23B H 0.4110 0.3845 0.0680 0.272 Uiso 1 1 calc R U . . .
H23C H 0.3807 0.4744 0.0685 0.272 Uiso 1 1 calc R U . . .
N3 N 0.5683(3) 0.26275(15) 0.32732(17) 0.0358(7) Uani 1 1 d . . . . .
C3 C 0.6575(3) 0.1996(2) 0.3123(2) 0.0435(9) Uani 1 1 d . . . . .
C31 C 0.5926(4) 0.1228(2) 0.3242(3) 0.0586(11) Uani 1 1 d . . . . .
H31A H 0.5768 0.1175 0.3826 0.088 Uiso 1 1 calc R U . . .
H31B H 0.6485 0.0810 0.3098 0.088 Uiso 1 1 calc R U . . .
H31C H 0.5108 0.1204 0.2878 0.088 Uiso 1 1 calc R U . . .
C32 C 0.7813(4) 0.2040(3) 0.3727(3) 0.0709(14) Uani 1 1 d . . . . .
H32A H 0.7613 0.1980 0.4301 0.106 Uiso 1 1 calc R U . . .
H32B H 0.8224 0.2539 0.3668 0.106 Uiso 1 1 calc R U . . .
H32C H 0.8397 0.1630 0.3598 0.106 Uiso 1 1 calc R U . . .
C33 C 0.6891(5) 0.2053(3) 0.2229(3) 0.0735(14) Uani 1 1 d . . . . .
H33A H 0.6099 0.2015 0.1842 0.110 Uiso 1 1 calc R U . . .
H33B H 0.7473 0.1636 0.2120 0.110 Uiso 1 1 calc R U . . .
H33C H 0.7306 0.2547 0.2150 0.110 Uiso 1 1 calc R U . . .
N4 N 0.5350(3) 0.36738(16) 0.40315(17) 0.0410(7) Uani 1 1 d . . . . .
C4 C 0.5168(3) 0.4331(2) 0.4504(2) 0.0419(9) Uani 1 1 d . . . . .
C5 C 0.4385(4) 0.4330(2) 0.5147(2) 0.0475(9) Uani 1 1 d . . . . .
H5 H 0.3950 0.3871 0.5260 0.057 Uiso 1 1 calc R U . . .
C6 C 0.5779(4) 0.5024(2) 0.4376(2) 0.0503(10) Uani 1 1 d . . . . .
H6 H 0.6326 0.5054 0.3949 0.060 Uiso 1 1 calc R U . . .
O1 O 0.1815(3) 0.34007(16) 0.23497(18) 0.0616(8) Uani 1 1 d . . . . .
C7 C 0.1486(4) 0.4028(3) 0.2872(3) 0.0703(13) Uani 1 1 d . . . . .
H7A H 0.1951 0.4500 0.2747 0.084 Uiso 1 1 calc R U . . .
H7B H 0.1708 0.3901 0.3471 0.084 Uiso 1 1 calc R U . . .
C8 C 0.0057(5) 0.4137(4) 0.2667(5) 0.111(2) Uani 1 1 d . . . . .
H8A H -0.0414 0.3845 0.3059 0.133 Uiso 1 1 calc R U . . .
H8B H -0.0175 0.4685 0.2695 0.133 Uiso 1 1 calc R U . . .
C9 C -0.0236(6) 0.3844(4) 0.1816(4) 0.113(2) Uani 1 1 d . . . . .
H9A H -0.0153 0.4255 0.1403 0.136 Uiso 1 1 calc R U . . .
H9B H -0.1121 0.3638 0.1725 0.136 Uiso 1 1 calc R U . . .
C10 C 0.0727(5) 0.3222(3) 0.1739(4) 0.0934(19) Uani 1 1 d . . . . .
H10A H 0.0364 0.2716 0.1857 0.112 Uiso 1 1 calc R U . . .
H10B H 0.0987 0.3214 0.1169 0.112 Uiso 1 1 calc R U . . .
O2 O 0.3227(3) 0.20841(15) 0.17157(16) 0.0548(7) Uani 1 1 d . . . . .
C14 C 0.2550(5) 0.1363(3) 0.1755(3) 0.0757(14) Uani 1 1 d . . . . .
H14A H 0.1613 0.1439 0.1621 0.091 Uiso 1 1 calc R U . . .
H14B H 0.2724 0.1134 0.2319 0.091 Uiso 1 1 calc R U . . .
C15 C 0.3049(6) 0.0866(3) 0.1124(3) 0.0975(19) Uani 1 1 d . . . . .
H15A H 0.2378 0.0506 0.0878 0.117 Uiso 1 1 calc R U . . .
H15B H 0.3798 0.0567 0.1379 0.117 Uiso 1 1 calc R U . . .
C16 C 0.3428(6) 0.1400(3) 0.0477(3) 0.0872(16) Uani 1 1 d . . . . .
H16A H 0.4281 0.1260 0.0320 0.105 Uiso 1 1 calc R U . . .
H16B H 0.2794 0.1384 -0.0030 0.105 Uiso 1 1 calc R U . . .
C17 C 0.3468(5) 0.2176(3) 0.0862(3) 0.0740(14) Uani 1 1 d . . . . .
H17A H 0.4320 0.2414 0.0840 0.089 Uiso 1 1 calc R U . . .
H17B H 0.2806 0.2510 0.0558 0.089 Uiso 1 1 calc R U . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 N2 2.061(3) . ?
Mg1 O2 2.061(3) . ?
Mg1 N1 2.062(3) . ?
Mg1 O1 2.079(3) . ?
Mg1 N3 2.337(3) . ?
Mg1 P1 2.8261(14) . ?
Mg1 P2 2.8345(15) . ?
P1 N1 1.648(3) . ?
P1 N4 1.745(3) . ?
P1 N3 1.778(3) . ?
P2 N2 1.647(3) . ?
P2 N4 1.757(3) . ?
P2 N3 1.767(3) . ?
N1 C1 1.484(5) . ?
C1 C13 1.522(6) . ?
C1 C12 1.529(5) . ?
C1 C11 1.536(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N2 C2 1.477(4) . ?
C2 C21 1.489(6) . ?
C2 C23 1.490(7) . ?
C2 C22 1.515(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N3 C3 1.486(4) . ?
C3 C33 1.520(6) . ?
C3 C31 1.526(5) . ?
C3 C32 1.528(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N4 C4 1.403(4) . ?
C4 C6 1.396(5) . ?
C4 C5 1.398(5) . ?
C5 C6 1.387(5) 3_666 ?
C5 H5 0.9500 . ?
C6 C5 1.387(5) 3_666 ?
C6 H6 0.9500 . ?
O1 C7 1.449(5) . ?
O1 C10 1.449(5) . ?
C7 C8 1.508(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.461(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.499(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O2 C17 1.438(5) . ?
O2 C14 1.450(5) . ?
C14 C15 1.479(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.489(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.489(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Mg1 O2 113.23(12) . . ?
N2 Mg1 N1 122.47(12) . . ?
O2 Mg1 N1 117.20(12) . . ?
N2 Mg1 O1 103.83(13) . . ?
O2 Mg1 O1 92.08(12) . . ?
N1 Mg1 O1 100.24(13) . . ?
N2 Mg1 N3 70.41(11) . . ?
O2 Mg1 N3 105.50(11) . . ?
N1 Mg1 N3 71.11(11) . . ?
O1 Mg1 N3 162.39(12) . . ?
N2 Mg1 P1 91.21(9) . . ?
O2 Mg1 P1 127.71(9) . . ?
N1 Mg1 P1 35.21(8) . . ?
O1 Mg1 P1 127.43(10) . . ?
N3 Mg1 P1 38.86(7) . . ?
N2 Mg1 P2 35.02(8) . . ?
O2 Mg1 P2 125.27(10) . . ?
N1 Mg1 P2 91.36(9) . . ?
O1 Mg1 P2 129.73(9) . . ?
N3 Mg1 P2 38.46(7) . . ?
P1 Mg1 P2 57.28(3) . . ?
N1 P1 N4 106.86(15) . . ?
N1 P1 N3 96.98(14) . . ?
N4 P1 N3 79.27(13) . . ?
N1 P1 Mg1 46.17(10) . . ?
N4 P1 Mg1 79.39(10) . . ?
N3 P1 Mg1 55.52(9) . . ?
N2 P2 N4 106.61(15) . . ?
N2 P2 N3 96.32(14) . . ?
N4 P2 N3 79.27(13) . . ?
N2 P2 Mg1 45.87(10) . . ?
N4 P2 Mg1 78.97(10) . . ?
N3 P2 Mg1 55.34(9) . . ?
C1 N1 P1 119.6(2) . . ?
C1 N1 Mg1 140.2(2) . . ?
P1 N1 Mg1 98.62(14) . . ?
N1 C1 C13 108.3(3) . . ?
N1 C1 C12 112.9(3) . . ?
C13 C1 C12 107.9(4) . . ?
N1 C1 C11 110.9(3) . . ?
C13 C1 C11 108.2(4) . . ?
C12 C1 C11 108.4(4) . . ?
C1 C11 H11A 109.5 . . ?
C1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C1 C12 H12A 109.5 . . ?
C1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 C13 H13A 109.5 . . ?
C1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2 N2 P2 120.9(3) . . ?
C2 N2 Mg1 139.6(3) . . ?
P2 N2 Mg1 99.11(14) . . ?
N2 C2 C21 112.2(3) . . ?
N2 C2 C23 109.3(4) . . ?
C21 C2 C23 108.3(5) . . ?
N2 C2 C22 111.7(4) . . ?
C21 C2 C22 106.1(5) . . ?
C23 C2 C22 109.2(6) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22A 109.5 . . ?
C2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 C23 H23A 109.5 . . ?
C2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C3 N3 P2 122.4(2) . . ?
C3 N3 P1 121.9(2) . . ?
P2 N3 P1 99.88(14) . . ?
C3 N3 Mg1 130.6(2) . . ?
P2 N3 Mg1 86.20(11) . . ?
P1 N3 Mg1 85.61(11) . . ?
N3 C3 C33 108.6(3) . . ?
N3 C3 C31 109.3(3) . . ?
C33 C3 C31 109.2(3) . . ?
N3 C3 C32 111.3(3) . . ?
C33 C3 C32 109.5(4) . . ?
C31 C3 C32 108.8(3) . . ?
C3 C31 H31A 109.5 . . ?
C3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C3 C32 H32A 109.5 . . ?
C3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C3 C33 H33A 109.5 . . ?
C3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 N4 P1 129.7(2) . . ?
C4 N4 P2 128.7(2) . . ?
P1 N4 P2 101.58(15) . . ?
C6 C4 C5 115.6(3) . . ?
C6 C4 N4 122.2(3) . . ?
C5 C4 N4 122.2(3) . . ?
C6 C5 C4 122.2(3) 3_666 . ?
C6 C5 H5 118.9 3_666 . ?
C4 C5 H5 118.9 . . ?
C5 C6 C4 122.1(4) 3_666 . ?
C5 C6 H6 118.9 3_666 . ?
C4 C6 H6 118.9 . . ?
C7 O1 C10 109.5(3) . . ?
C7 O1 Mg1 117.5(2) . . ?
C10 O1 Mg1 132.8(3) . . ?
O1 C7 C8 105.5(4) . . ?
O1 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
O1 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.8 . . ?
C9 C8 C7 104.7(5) . . ?
C9 C8 H8A 110.8 . . ?
C7 C8 H8A 110.8 . . ?
C9 C8 H8B 110.8 . . ?
C7 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?
C8 C9 C10 105.3(5) . . ?
C8 C9 H9A 110.7 . . ?
C10 C9 H9A 110.7 . . ?
C8 C9 H9B 110.7 . . ?
C10 C9 H9B 110.7 . . ?
H9A C9 H9B 108.8 . . ?
O1 C10 C9 105.8(4) . . ?
O1 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
O1 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
C17 O2 C14 106.4(3) . . ?
C17 O2 Mg1 124.6(2) . . ?
C14 O2 Mg1 128.6(3) . . ?
O2 C14 C15 105.2(4) . . ?
O2 C14 H14A 110.7 . . ?
C15 C14 H14A 110.7 . . ?
O2 C14 H14B 110.7 . . ?
C15 C14 H14B 110.7 . . ?
H14A C14 H14B 108.8 . . ?
C14 C15 C16 105.2(4) . . ?
C14 C15 H15A 110.7 . . ?
C16 C15 H15A 110.7 . . ?
C14 C15 H15B 110.7 . . ?
C16 C15 H15B 110.7 . . ?
H15A C15 H15B 108.8 . . ?
C17 C16 C15 105.8(4) . . ?
C17 C16 H16A 110.6 . . ?
C15 C16 H16A 110.6 . . ?
C17 C16 H16B 110.6 . . ?
C15 C16 H16B 110.6 . . ?
H16A C16 H16B 108.7 . . ?
O2 C17 C16 107.3(4) . . ?
O2 C17 H17A 110.2 . . ?
C16 C17 H17A 110.2 . . ?
O2 C17 H17B 110.2 . . ?
C16 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 P1 N1 C1 -135.3(3) . . . . ?
N3 P1 N1 C1 143.9(3) . . . . ?
Mg1 P1 N1 C1 168.6(3) . . . . ?
N4 P1 N1 Mg1 56.11(16) . . . . ?
N3 P1 N1 Mg1 -24.74(15) . . . . ?
P1 N1 C1 C13 177.0(3) . . . . ?
Mg1 N1 C1 C13 -20.7(5) . . . . ?
P1 N1 C1 C12 57.6(4) . . . . ?
Mg1 N1 C1 C12 -140.1(3) . . . . ?
P1 N1 C1 C11 -64.3(4) . . . . ?
Mg1 N1 C1 C11 98.0(4) . . . . ?
N4 P2 N2 C2 119.1(3) . . . . ?
N3 P2 N2 C2 -160.3(3) . . . . ?
Mg1 P2 N2 C2 174.5(4) . . . . ?
N4 P2 N2 Mg1 -55.42(16) . . . . ?
N3 P2 N2 Mg1 25.23(15) . . . . ?
P2 N2 C2 C21 -71.5(5) . . . . ?
Mg1 N2 C2 C21 100.1(5) . . . . ?
P2 N2 C2 C23 168.5(5) . . . . ?
Mg1 N2 C2 C23 -20.0(7) . . . . ?
P2 N2 C2 C22 47.5(6) . . . . ?
Mg1 N2 C2 C22 -141.0(5) . . . . ?
N2 P2 N3 C3 115.1(3) . . . . ?
N4 P2 N3 C3 -139.2(3) . . . . ?
Mg1 P2 N3 C3 136.9(3) . . . . ?
N2 P2 N3 P1 -106.71(15) . . . . ?
N4 P2 N3 P1 -0.94(14) . . . . ?
Mg1 P2 N3 P1 -84.87(12) . . . . ?
N2 P2 N3 Mg1 -21.84(14) . . . . ?
N4 P2 N3 Mg1 83.94(12) . . . . ?
N1 P1 N3 C3 -114.6(3) . . . . ?
N4 P1 N3 C3 139.5(3) . . . . ?
Mg1 P1 N3 C3 -136.1(3) . . . . ?
N1 P1 N3 P2 106.85(15) . . . . ?
N4 P1 N3 P2 0.94(14) . . . . ?
Mg1 P1 N3 P2 85.37(12) . . . . ?
N1 P1 N3 Mg1 21.48(13) . . . . ?
N4 P1 N3 Mg1 -84.43(12) . . . . ?
P2 N3 C3 C33 -54.5(4) . . . . ?
P1 N3 C3 C33 176.1(3) . . . . ?
Mg1 N3 C3 C33 61.7(4) . . . . ?
P2 N3 C3 C31 -173.6(2) . . . . ?
P1 N3 C3 C31 57.0(4) . . . . ?
Mg1 N3 C3 C31 -57.5(4) . . . . ?
P2 N3 C3 C32 66.2(4) . . . . ?
P1 N3 C3 C32 -63.2(4) . . . . ?
Mg1 N3 C3 C32 -177.7(3) . . . . ?
N1 P1 N4 C4 87.0(3) . . . . ?
N3 P1 N4 C4 -178.8(3) . . . . ?
Mg1 P1 N4 C4 124.6(3) . . . . ?
N1 P1 N4 P2 -95.08(17) . . . . ?
N3 P1 N4 P2 -0.95(14) . . . . ?
Mg1 P1 N4 P2 -57.54(12) . . . . ?
N2 P2 N4 C4 -87.7(3) . . . . ?
N3 P2 N4 C4 178.9(3) . . . . ?
Mg1 P2 N4 C4 -124.7(3) . . . . ?
N2 P2 N4 P1 94.42(17) . . . . ?
N3 P2 N4 P1 0.96(14) . . . . ?
Mg1 P2 N4 P1 57.40(12) . . . . ?
P1 N4 C4 C6 162.9(3) . . . . ?
P2 N4 C4 C6 -14.4(5) . . . . ?
P1 N4 C4 C5 -15.6(5) . . . . ?
P2 N4 C4 C5 167.0(3) . . . . ?
C6 C4 C5 C6 0.3(6) . . . 3_666 ?
N4 C4 C5 C6 178.9(4) . . . 3_666 ?
C5 C4 C6 C5 -0.3(6) . . . 3_666 ?
N4 C4 C6 C5 -178.9(4) . . . 3_666 ?
C10 O1 C7 C8 10.5(6) . . . . ?
Mg1 O1 C7 C8 -166.1(4) . . . . ?
O1 C7 C8 C9 -25.7(6) . . . . ?
C7 C8 C9 C10 30.7(7) . . . . ?
C7 O1 C10 C9 8.4(6) . . . . ?
Mg1 O1 C10 C9 -175.7(4) . . . . ?
C8 C9 C10 O1 -24.6(7) . . . . ?
C17 O2 C14 C15 32.1(5) . . . . ?
Mg1 O2 C14 C15 -154.5(3) . . . . ?
O2 C14 C15 C16 -28.7(6) . . . . ?
C14 C15 C16 C17 14.8(6) . . . . ?
C14 O2 C17 C16 -22.7(5) . . . . ?
Mg1 O2 C17 C16 163.5(3) . . . . ?
C15 C16 C17 O2 4.5(6) . . . . ?




