# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_fb144ht_cr1
_database_code_depnum_ccdc_archive 'CCDC 1956355'
loop_
_audit_author_name
_audit_author_address
Perez
;CRISMAT
France
;
_audit_update_record             
;
2019-09-27 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
_audit_creation_date             2019-09-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        'copper 6-hydroxy-2-naphtylphosphonate hydrate'
_chemical_formula_moiety         'C20 H18 Cu2 O10 P2, 0.5(H4 O2)'
_chemical_formula_sum            'C20 H20 Cu2 O11 P2'
_chemical_formula_weight         625.38
_chemical_melting_point          ?
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   5.66017(4)
_cell_length_b                   4.75153(4)
_cell_length_c                   41.0950(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.0499(6)
_cell_angle_gamma                90
_cell_volume                     1103.662(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.4440
_cell_measurement_theta_min      4.2850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0089
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            26244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.872
_diffrn_reflns_theta_min         4.310
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Eiger 1M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     18.00 114.00   0.40   30.00    --   43.75  19.00  60.00  240
  2  ω     65.00  91.00   0.40   30.00    --   43.75  77.00 -30.00   65
  3  ω    105.00 130.20   0.40   30.00    --  110.00 137.00 -51.00   63
  4  ω    113.00 152.20   0.40   30.00    --  110.00 125.00 -60.00   98
  5  ω    134.00 160.00   0.40   30.00    --  110.00 125.00 -90.00   65
  6  ω    120.00 167.20   0.40   30.00    --  110.00  77.00 -30.00  118
  7  ω    127.00 153.00   0.40   30.00    --  110.00  15.00 -90.00   65
  8  ω    120.00 145.20   0.40   30.00    --  110.00  45.00 -30.00   63
  9  ω    113.00 139.00   0.40   30.00    --  110.00 -15.00   0.00   65
 10  ω    111.00 137.00   0.40   30.00    --  110.00 -15.00  60.00   65
 11  ω     96.00 122.00   0.40   30.00    --  110.00 -45.00 120.00   65
 12  ω     93.00 129.00   0.40   30.00    --  110.00 -61.00  90.00   90
 13  ω     86.00 112.00   0.40   30.00    --  110.00 -45.00  30.00   65
 14  ω     64.00  98.00   0.40   30.00    --  110.00 -94.00  90.00   85
 15  ω     55.00  80.20   0.40   30.00    --  110.00-132.00  62.00   63
 16  ω     59.00  96.20   0.40   30.00    --  110.00 -94.00  60.00   93
 17  ω     57.00  82.20   0.40   30.00    --  110.00 -45.00 120.00   63
 18  ω     51.00  80.20   0.40   30.00    --  110.00 -45.00  30.00   73
 19  ω     59.00  90.20   0.40   30.00    --  110.00 -15.00   0.00   78
 20  ω     59.00  85.00   0.40   30.00    --  110.00 -30.00 -60.00   65
 21  ω     98.00 130.00   0.40   30.00    --  110.00 -61.00-120.00   80
 22  ω     79.00 110.20   0.40   30.00    --  110.00-125.00-180.00   78
 23  ω     69.00  94.20   0.40   30.00    --  110.00-137.00-114.00   63
 24  ω     71.00 103.00   0.40   30.00    --  110.00-125.00 -90.00   80
 25  ω     68.00 133.20   0.40   30.00    --  110.00 -77.00-120.00  163
 26  ω     77.00 127.00   0.40   30.00    --  110.00 -30.00-120.00  125
 27  ω    127.00 153.00   0.40   30.00    --  110.00  15.00-180.00   65
 28  ω     99.00 131.00   0.40   30.00    --  110.00  45.00-120.00   80
 29  ω     97.00 170.20   0.40   30.00    --  110.00  45.00 -60.00  183
 30  ω    104.00 170.00   0.40   30.00    --  110.00  61.00  30.00  165
 31  ω    110.00 147.20   0.40   30.00    --  110.00  30.00  60.00   93
 32  ω     82.00 113.20   0.40   30.00    --  110.00  77.00 -60.00   78
 33  ω     86.00 168.00   0.40   30.00    --  110.00  77.00-120.00  205
 34  ω    105.00 156.20   0.40   30.00    --  110.00 125.00-180.00  128
 35  ω     94.00 162.00   0.40   30.00    --  110.00 125.00-120.00  170
 36  ω     91.00 147.00   0.40   30.00    --  110.00 132.00 131.00  140
 37  ω     16.00 107.20   0.40   30.00    --   43.75  77.00 -90.00  228
 38  ω     35.00  64.20   0.40   30.00    --  110.00 -30.00-120.00   73
 39  ω     66.00 122.00   0.40   30.00    --  110.00 -45.00-150.00  140
 40  ω     73.00 132.20   0.40   30.00    --  110.00 -77.00-180.00  148
 41  ω     73.00 116.20   0.40   30.00    --  110.00 -61.00-150.00  108
 42  ω     49.00  86.20   0.40   30.00    --  110.00-125.00-150.00   93
 43  ω     43.00  71.00   0.40   30.00    --  110.00-125.00-180.00   70
 44  ω     39.00  66.20   0.40   30.00    --  110.00-125.00 -90.00   68
 45  ω     48.00  73.20   0.40   30.00    --  110.00 -45.00 -60.00   63
 46  ω     44.00 113.20   0.40   30.00    --  110.00 -61.00   0.00  173
 47  ω     58.00  89.20   0.40   30.00    --  110.00-125.00  90.00   78
 48  ω     43.00  88.20   0.40   30.00    --   43.75-132.00  62.00  113
 49  ω     13.00  54.20   0.40   30.00    --   43.75 -38.00  90.00  103
 50  ω    -27.00   5.00   0.40   30.00    --   43.75 -38.00  90.00   80
 51  ω     16.00  43.20   0.40   30.00    --   43.75  77.00 -30.00   68
 52  ω     32.00  65.20   0.40   30.00    --   43.75 -77.00-180.00   83
 53  ω     43.00  72.20   0.40   30.00    --   43.75-137.00-114.00   73
 54  ω     -2.00  29.20   0.40   30.00    --   -0.75 -94.00-120.00   78
 55  ω      6.00  33.20   0.40   30.00    --   -0.75 -94.00-180.00   68
 56  ω    -21.00  19.00   0.40   30.00    --   43.75 -77.00-180.00  100
 57  ω    112.00 138.00   0.40   30.00    --  110.00 132.00 131.00   65
 58  ω     15.00  49.00   0.40   30.00    --   43.75  77.00 150.00   85
 59  ω     27.00  53.00   0.40   30.00    --   43.75 -99.00   0.00   65
 60  ω     16.00  66.00   0.40   30.00    --   43.75  77.00 -60.00  125
 61  ω     69.00  98.20   0.40   30.00    --   43.75  77.00 150.00   73
 62  ω     65.00 103.00   0.40   30.00    --   43.75  77.00  30.00   95
 63  ω     82.00 107.20   0.40   30.00    --   43.75  77.00-150.00   63
 64  ω     16.00  50.00   0.40   30.00    --   43.75  77.00-180.00   85
 65  ω     15.00  65.00   0.40   30.00    --   43.75  77.00-150.00  125
 66  ω    -20.00  15.20   0.40   30.00    --   43.75 -77.00 -60.00   88
 67  ω      0.00  53.20   0.40   30.00    --   43.75 -99.00  60.00  133
 68  ω     17.00  55.00   0.40   30.00    --   43.75  77.00  30.00   95
 69  ω     15.00  60.20   0.40   30.00    --   43.75  77.00  90.00  113
 70  ω     17.00  60.20   0.40   30.00    --   43.75  77.00   0.00  108
 71  ω     27.00  61.00   0.40   30.00    --   43.75 -77.00 -60.00   85
 72  ω     71.00 107.00   0.40   30.00    --   43.75  77.00  90.00   90
 73  ω     64.00 105.20   0.40   30.00    --   43.75  77.00-180.00  103
 74  ω     81.00 107.00   0.40   30.00    --  110.00  77.00 -90.00   65
 75  ω     81.00 145.00   0.40   30.00    --  110.00  77.00  90.00  160
 76  ω    131.00 171.00   0.40   30.00    --  110.00  61.00  60.00  100
 77  ω     81.00 106.20   0.40   30.00    --  110.00  77.00-150.00   63
 78  ω     85.00 111.00   0.40   30.00    --  110.00  77.00 -54.17   65
 79  ω    143.80 171.00   0.40   30.00    --  110.00  77.00  30.00   68
 80  ω     89.00 126.20   0.40   30.00    --  110.00  61.00  60.00   93
 81  ω     81.00 122.20   0.40   30.00    --  110.00  78.00 106.13  103
 82  ω    132.00 159.20   0.40   30.00    --  110.00  78.00 106.13   68
 83  ω     84.00 109.20   0.40   30.00    --  110.00  71.00   1.64   63
 84  ω     48.00  87.20   0.40   30.00    --  110.00 -45.00-180.00   98
 85  ω     81.00 120.20   0.40   30.00    --  110.00  78.00 171.77   98
 86  ω    141.00 167.00   0.40   30.00    --  110.00  78.00 171.77   65
 87  ω    139.00 170.20   0.40   30.00    --  110.00  72.00  19.22   78
 88  ω     83.00 109.00   0.40   30.00    --  110.00  72.00  19.22   65
 89  ω     81.00 107.00   0.40   30.00    --  110.00  77.00  30.00   65
 90  ω     89.00 115.00   0.40   30.00    --  110.00  61.00-150.00   65
 91  ω    145.00 170.20   0.40   30.00    --  110.00  30.00   0.00   63
 92  ω     80.00 106.00   0.40   30.00    --  110.00  80.00 -28.21   65
 93  ω     81.00 149.00   0.40   30.00    --  110.00  77.00 120.00  170
 94  ω     95.00 126.20   0.40   30.00    --  110.00  30.00   0.00   78
 95  ω    140.00 167.20   0.40   30.00    --  110.00  61.00  90.00   68
 96  ω     89.00 115.00   0.40   30.00    --  110.00  61.00  90.00   65
 97  ω     89.00 114.20   0.40   30.00    --  110.00  61.00 -90.00   63
 98  ω     81.00 125.00   0.40   30.00    --  110.00  77.00 140.28  110
 99  ω     81.00 107.00   0.40   30.00    --  110.00  77.00-120.00   65
100  ω     89.00 115.00   0.40   30.00    --  110.00  61.00   0.00   65
101  ω     89.00 114.20   0.40   30.00    --  110.00  61.00-180.00   63
102  ω    125.00 166.20   0.40   30.00    --  110.00  61.00-180.00  103
103  ω     83.00 113.00   0.40   30.00    --  110.00  74.00-143.23   75
104  ω     81.00 106.20   0.40   30.00    --  110.00  77.00 -30.00   63
105  ω    134.00 160.00   0.40   30.00    --  110.00  77.00 -30.00   65
106  ω     99.00 151.00   0.40   30.00    --  110.00  45.00-150.00  130
107  ω     94.00 120.00   0.40   30.00    --  110.00  30.00 -30.00   65
108  ω    139.00 165.00   0.40   30.00    --  110.00  61.00 -60.00   65
109  ω     82.00 132.00   0.40   30.00    --  110.00  77.00 154.12  125
110  ω     81.00 146.20   0.40   30.00    --  110.00  77.00  60.00  163
111  ω     89.00 114.20   0.40   30.00    --  110.00  61.00 -60.00   63
112  ω     82.00 108.00   0.40   30.00    --  110.00  77.00-180.00   65
113  ω    134.00 160.00   0.40   30.00    --  110.00  71.00   1.64   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2269
_reflns_number_total             2278
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00061(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2278
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0374
_refine_ls_restrained_S_all      1.264
_refine_ls_shift/su_max          2.955
_refine_ls_shift/su_mean         0.068
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²+3.8156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0965
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: C1A(0.5) H1A(0.5) C2A(0.5) H2A(0.5) C2B(0.5) H2B(0.5) C3B(0.5)
 H3B(0.5) C8B(0.5) H8B(0.5) C8A(0.5) H8A(0.5) C7B(0.5) H7B(0.5) C7A(0.5)
 H7A(0.5) O5(0.5) H5A(0.5) H5B(0.5)
3.a Free rotating group:
 O5(H5A,H5B)
3.b Rotating group:
 O6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C5(H5), C1A(H1A), C2A(H2A), C2B(H2B), C3B(H3B), C8B(H8B), C8A(H8A),
 C7B(H7B), C7A(H7A)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Cu1 Cu 1.00666(7) 0.20476(10) 0.25603(2) 0.01622(16) Uani 1 1 d . . . . .
P1 P 0.54353(13) 0.26576(17) 0.29054(2) 0.01441(19) Uani 1 1 d . . . . .
O3 O 0.3367(3) 0.4329(5) 0.27385(5) 0.0164(4) Uani 1 1 d . . . . .
O2 O 0.5306(4) -0.0434(5) 0.28227(5) 0.0195(5) Uani 1 1 d . . . . .
O1 O 0.7751(4) 0.4030(5) 0.28071(5) 0.0189(5) Uani 1 1 d . . . . .
O6 O 1.0350(4) -0.0875(5) 0.29160(5) 0.0205(5) Uani 1 1 d . . . . .
H6A H 1.158815 -0.195490 0.289349 0.031 Uiso 1 1 d GR . . . .
H6B H 0.916998 -0.207088 0.289798 0.031 Uiso 1 1 d GR . . . .
C1 C 0.5257(6) 0.3008(8) 0.33376(8) 0.0226(7) Uani 1 1 d . . . . .
C9 C 0.3491(9) 0.4929(12) 0.38116(10) 0.0542(14) Uani 1 1 d . . . . .
C10 C 0.3608(10) 0.4567(14) 0.34730(10) 0.0657(18) Uani 1 1 d . . . . .
H10 H 0.247852 0.545837 0.333638 0.079 Uiso 1 1 calc R . . . .
C4 C 0.5043(9) 0.3557(13) 0.40164(10) 0.0552(14) Uani 1 1 d . . . . .
O4 O 0.2992(11) 0.5815(15) 0.48096(9) 0.113(2) Uani 1 1 d . . . . .
H4 H 0.386502 0.707522 0.488059 0.169 Uiso 1 1 calc GR . . . .
C6 C 0.3221(12) 0.5541(16) 0.44824(12) 0.0726(19) Uani 1 1 d . . . . .
C5 C 0.4902(14) 0.3892(19) 0.43601(12) 0.097(3) Uani 1 1 d . . . . .
H5 H 0.597984 0.296443 0.450126 0.116 Uiso 1 1 calc R . . . .
C1A C 0.7272(15) 0.242(2) 0.35425(19) 0.0320(17) Uani 0.5 1 d . . P A 2
H1A H 0.864286 0.177510 0.345173 0.038 Uiso 0.5 1 calc R . P A 2
C2A C 0.7247(16) 0.277(2) 0.3872(2) 0.042(2) Uani 0.5 1 d . . P A 2
H2A H 0.862171 0.251801 0.400260 0.051 Uiso 0.5 1 calc R . P A 2
C2B C 0.6331(19) 0.087(2) 0.3548(2) 0.041(2) Uani 0.5 1 d . . P A 1
H2B H 0.711950 -0.064164 0.345904 0.049 Uiso 0.5 1 calc R . P A 1
C3B C 0.618(2) 0.108(2) 0.3878(2) 0.051(3) Uani 0.5 1 d . . P A 1
H3B H 0.678908 -0.033266 0.401384 0.061 Uiso 0.5 1 calc R . P A 1
C8B C 0.235(2) 0.737(2) 0.3955(2) 0.052(3) Uani 0.5 1 d . . P B 1
H8B H 0.175784 0.879736 0.381890 0.063 Uiso 0.5 1 calc R . P B 1
C8A C 0.118(2) 0.570(3) 0.3948(3) 0.059(3) Uani 0.5 1 d . . P B 2
H8A H -0.019635 0.586746 0.381652 0.071 Uiso 0.5 1 calc R . P B 2
C7B C 0.215(3) 0.758(3) 0.4274(4) 0.062(4) Uani 0.5 1 d . . P B 1
H7B H 0.131509 0.906600 0.435959 0.075 Uiso 0.5 1 calc R . P B 1
C7A C 0.121(3) 0.616(4) 0.4280(4) 0.083(6) Uani 0.5 1 d . . P B 2
H7A H -0.013147 0.689580 0.437070 0.100 Uiso 0.5 1 calc R . P B 2
O5 O 0.443(9) 0.562(9) -0.0005(13) 0.183(13) Uani 0.5 1 d . . P . .
H5A H 0.340438 0.715622 -0.006787 2(3) Uiso 0.5 1 d G . P . .
H5B H 0.393506 0.411790 -0.014887 0.9(4) Uiso 0.5 1 d G . P . .


_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
Cu1 P1 2.8348(9) 2_645 ?
Cu1 O3 2.019(2) 2_645 ?
Cu1 O3 2.248(2) 1_655 ?
Cu1 O2 1.979(2) 2_655 ?
Cu1 O1 1.943(2) . ?
Cu1 O6 2.017(2) . ?
P1 O3 1.545(2) . ?
P1 O2 1.509(2) . ?
P1 O1 1.537(2) . ?
P1 C1 1.792(3) . ?
O6 H6A 0.8774 . ?
O6 H6B 0.8769 . ?
C1 C10 1.336(5) . ?
C1 C1A 1.410(8) . ?
C1 C2B 1.447(9) . ?
C9 C10 1.407(6) . ?
C9 C4 1.352(6) . ?
C9 C8B 1.464(10) . ?
C9 C8A 1.495(11) . ?
C10 H10 0.9300 . ?
C4 C5 1.428(6) . ?
C4 C2A 1.459(10) . ?
C4 C3B 1.469(11) . ?
O4 H4 0.8203 . ?
O4 C6 1.364(6) . ?
C6 C5 1.350(8) . ?
C6 C7B 1.408(17) . ?
C6 C7A 1.407(19) . ?
C5 H5 0.9300 . ?
C1A H1A 0.9300 . ?
C1A C2A 1.364(11) . ?
C2A H2A 0.9300 . ?
C2B H2B 0.9300 . ?
C2B C3B 1.367(12) . ?
C3B H3B 0.9300 . ?
C8B H8B 0.9300 . ?
C8B C7B 1.327(17) . ?
C8A H8A 0.9300 . ?
C8A C7A 1.378(19) . ?
C7B H7B 0.9300 . ?
C7A H7A 0.9300 . ?
O5 O5 0.87(5) 3_665 ?
O5 H5A 0.9582 . ?
O5 H5B 0.9593 . ?

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
O3 Cu1 P1 128.78(6) 1_655 2_645 ?
O3 Cu1 P1 31.83(6) 2_645 2_645 ?
O3 Cu1 O3 97.03(5) 2_645 1_655 ?
O2 Cu1 P1 84.57(7) 2_655 2_645 ?
O2 Cu1 O3 86.27(9) 2_655 2_645 ?
O2 Cu1 O3 91.10(9) 2_655 1_655 ?
O2 Cu1 O6 173.58(10) 2_655 . ?
O1 Cu1 P1 131.53(7) . 2_645 ?
O1 Cu1 O3 163.27(9) . 2_645 ?
O1 Cu1 O3 99.67(9) . 1_655 ?
O1 Cu1 O2 94.35(10) . 2_655 ?
O1 Cu1 O6 89.15(9) . . ?
O6 Cu1 P1 89.07(7) . 2_645 ?
O6 Cu1 O3 88.83(9) . 2_645 ?
O6 Cu1 O3 93.63(8) . 1_655 ?
O3 P1 Cu1 43.59(8) . 2_655 ?
O3 P1 C1 108.12(14) . . ?
O2 P1 Cu1 124.23(9) . 2_655 ?
O2 P1 O3 111.96(12) . . ?
O2 P1 O1 112.68(13) . . ?
O2 P1 C1 108.01(15) . . ?
O1 P1 Cu1 64.33(9) . 2_655 ?
O1 P1 O3 107.59(12) . . ?
O1 P1 C1 108.34(14) . . ?
C1 P1 Cu1 126.28(12) . 2_655 ?
Cu1 O3 Cu1 119.63(9) 2_655 1_455 ?
P1 O3 Cu1 104.58(11) . 2_655 ?
P1 O3 Cu1 119.59(12) . 1_455 ?
P1 O2 Cu1 140.32(14) . 2_645 ?
P1 O1 Cu1 122.68(14) . . ?
Cu1 O6 H6A 111.1 . . ?
Cu1 O6 H6B 110.7 . . ?
H6A O6 H6B 102.8 . . ?
C10 C1 P1 122.8(3) . . ?
C10 C1 C1A 115.0(5) . . ?
C10 C1 C2B 114.9(5) . . ?
C1A C1 P1 119.1(4) . . ?
C2B C1 P1 118.8(4) . . ?
C10 C9 C8B 122.6(6) . . ?
C10 C9 C8A 119.3(6) . . ?
C4 C9 C10 119.6(4) . . ?
C4 C9 C8B 114.7(6) . . ?
C4 C9 C8A 115.9(6) . . ?
C1 C10 C9 123.4(4) . . ?
C1 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C9 C4 C5 119.6(5) . . ?
C9 C4 C2A 114.3(5) . . ?
C9 C4 C3B 115.3(5) . . ?
C5 C4 C2A 121.7(5) . . ?
C5 C4 C3B 121.4(6) . . ?
C6 O4 H4 109.6 . . ?
O4 C6 C7B 118.3(8) . . ?
O4 C6 C7A 116.6(8) . . ?
C5 C6 O4 121.9(6) . . ?
C5 C6 C7B 117.5(7) . . ?
C5 C6 C7A 117.8(8) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.7(5) . . ?
C6 C5 H5 119.7 . . ?
C1 C1A H1A 119.4 . . ?
C2A C1A C1 121.1(7) . . ?
C2A C1A H1A 119.4 . . ?
C4 C2A H2A 120.3 . . ?
C1A C2A C4 119.4(7) . . ?
C1A C2A H2A 120.3 . . ?
C1 C2B H2B 120.2 . . ?
C3B C2B C1 119.5(8) . . ?
C3B C2B H2B 120.2 . . ?
C4 C3B H3B 120.1 . . ?
C2B C3B C4 119.8(8) . . ?
C2B C3B H3B 120.1 . . ?
C9 C8B H8B 119.4 . . ?
C7B C8B C9 121.3(10) . . ?
C7B C8B H8B 119.4 . . ?
C9 C8A H8A 121.7 . . ?
C7A C8A C9 116.6(11) . . ?
C7A C8A H8A 121.7 . . ?
C6 C7B H7B 120.2 . . ?
C8B C7B C6 119.5(12) . . ?
C8B C7B H7B 120.2 . . ?
C6 C7A H7A 119.4 . . ?
C8A C7A C6 121.1(12) . . ?
C8A C7A H7A 119.5 . . ?
O5 O5 H5A 164.3 3_665 . ?
O5 O5 H5B 73.6 3_665 . ?
H5A O5 H5B 104.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_fb316cristal2_col
_database_code_depnum_ccdc_archive 'CCDC 1956356'
loop_
_audit_author_name
_audit_author_address
Perez
;CRISMAT
France
;
_audit_update_record             
;
2019-09-27 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
_audit_creation_date             2018-10-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'cobalt 6-hydroxy-2-naphtylphosphonate hydrate'
_chemical_formula_moiety         'C20 H18 Co2 O10 P2, H2 O'
_chemical_formula_sum            'C20 H20 Co2 O11 P2'
_chemical_formula_weight         616.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co1 P1 C10 O4 H11'
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'
Co Co 0.3494 0.9721 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.3353(3)
_cell_length_b                   40.691(2)
_cell_length_c                   7.4400(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.144(4)
_cell_angle_gamma                90
_cell_volume                     2192.50(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.9520
_cell_measurement_theta_min      2.9260
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.782
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            39912
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.134
_diffrn_reflns_theta_min         2.813
_diffrn_ambient_temperature      293
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.33 140.83   0.50   40.00    --   35.00 175.00  30.00  203
  2  φ   -360.00   9.00   0.50   40.00 -38.81 -25.00 175.00    --   738
  3  ω     39.69 100.69   0.50   40.00    --   40.00 175.00 120.00  122
  4  ω     39.33 140.83   0.50   40.00    --   35.00 175.00 -25.00  203
  5  ω     39.63 134.63   0.50   40.00    --   40.00 175.00 -60.00  190
  6  ω     39.75 121.25   0.50   40.00    --   40.00 175.00 150.00  163
  7  ω     39.33 130.83   0.50   40.00    --   25.00 175.00-170.00  183
  8  ω     98.33 145.83   0.50   40.00    --   40.00 175.00  50.00   95
  9  ω     39.39  74.39   0.50   40.00    --   35.00 175.00 -45.00   70
 10  ω     54.79  87.79   0.50   40.00    --   40.00 175.00 -65.00   66
 11  ω     39.52 106.02   0.50   40.00    --   30.00 175.00  60.00  133
 12  φ   -360.00   9.00   0.50   40.00 -38.98  20.00 175.00    --   738
;
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker Nonius four-circle  diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0931269000
_diffrn_orient_matrix_UB_12      -0.0025651000
_diffrn_orient_matrix_UB_13      -0.0405924000
_diffrn_orient_matrix_UB_21      -0.0137557000
_diffrn_orient_matrix_UB_22      0.0172388000
_diffrn_orient_matrix_UB_23      -0.0062531000
_diffrn_orient_matrix_UB_31      0.0270732000
_diffrn_orient_matrix_UB_32      -0.0000502000
_diffrn_orient_matrix_UB_33      -0.0873918000
_diffrn_radiation_collimation    .
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           600\mA
_diffrn_source_power             30W
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50kV
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4717
_reflns_number_total             7693
_reflns_odcompleteness_completeness 84.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.06
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         7693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²+7.4628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1137
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Free rotating group:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3C,H3D)
2.b Aromatic/amide H refined with riding coordinates:
 C2A(H2AA), C2B(H2BA), C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C7A(H7A),
 C7B(H7B), C8A(H8A), C8B(H8B), C10A(H10A), C10B(H10B)
2.c Tetrahedral OH refined with riding coordinates:
 O1A(H1AA), O1B(H1BA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Co1 Co 0.25965(5) 0.75475(2) 0.78640(5) 0.01280(8) Uani 1 1 d . . . . .
Co2 Co 0.75980(5) 0.75521(2) 0.28601(5) 0.01260(8) Uani 1 1 d . . . . .
P1A P 0.54359(9) 0.79082(2) 0.56954(8) 0.01114(13) Uani 1 1 d . . . . .
P1B P 1.04300(9) 0.70868(2) 0.56786(8) 0.01107(13) Uani 1 1 d . . . . .
O1 O 0.1103(3) 0.79289(5) 0.6378(3) 0.0186(4) Uani 1 1 d . . . A -1
H1A H -0.0168 0.7913 0.6526 0.10(2) Uiso 1 1 d G . . A -1
H1B H 0.1103 0.7879 0.5119 0.10(2) Uiso 1 1 d G . . A -1
O1A O 0.6677(7) 0.98252(8) 0.8861(5) 0.0788(13) Uani 1 1 d . . . . .
H1AA H 0.6699 0.9928 0.7915 0.118 Uiso 1 1 calc R . . . .
O1B O 1.1761(6) 0.51665(7) 0.8706(5) 0.0703(12) Uani 1 1 d . . . . .
H1BA H 1.1880 0.5122 0.9794 0.106 Uiso 1 1 calc R . . . .
O2 O 0.6138(3) 0.79381(5) 0.1386(3) 0.0182(4) Uani 1 1 d . . . B -1
H2A H 0.4838 0.7916 0.1391 0.068(16) Uiso 1 1 d G . . B -1
H2B H 0.6271 0.7916 0.0131 0.085(19) Uiso 1 1 d G . . B -1
O2A O 0.5069(3) 0.77512(5) 0.7498(2) 0.0144(4) Uani 1 1 d . . . . .
O2B O 1.2271(2) 0.72400(5) 0.5323(2) 0.0149(4) Uani 1 1 d . . . . .
O3A O 0.3875(3) 0.78572(5) 0.4138(2) 0.0150(4) Uani 1 1 d . . . . .
O3B O 1.0088(2) 0.72415(5) 0.7497(2) 0.0141(4) Uani 1 1 d . . . . .
O4A O 0.7266(2) 0.77523(5) 0.5330(2) 0.0142(4) Uani 1 1 d . . . . .
O4B O 0.8872(3) 0.71440(5) 0.4127(2) 0.0147(4) Uani 1 1 d . . . . .
C1A C 0.5800(4) 0.83383(7) 0.6052(4) 0.0168(5) Uani 1 1 d . . . . .
C1B C 1.0687(4) 0.66519(7) 0.5986(4) 0.0162(5) Uani 1 1 d . . . . .
C2A C 0.6543(5) 0.85284(8) 0.4740(4) 0.0291(7) Uani 1 1 d . . . . .
H2AA H 0.6825 0.8428 0.3695 0.035 Uiso 1 1 calc R . . . .
C2B C 1.0395(6) 0.64375(8) 0.4470(4) 0.0354(8) Uani 1 1 d . . . . .
H2BA H 1.0091 0.6524 0.3304 0.043 Uiso 1 1 calc R . . . .
C3A C 0.6847(6) 0.88575(9) 0.5002(5) 0.0364(8) Uani 1 1 d . . . . .
H3A H 0.7322 0.8979 0.4125 0.044 Uiso 1 1 calc R . . . .
C3B C 1.0553(7) 0.61063(9) 0.4698(5) 0.0436(10) Uani 1 1 d . . . . .
H3B H 1.0358 0.5970 0.3683 0.052 Uiso 1 1 calc R . . . .
C4A C 0.6448(6) 0.90161(8) 0.6590(5) 0.0321(8) Uani 1 1 d . . . . .
C4B C 1.1010(5) 0.59653(8) 0.6451(5) 0.0312(7) Uani 1 1 d . . . . .
C5A C 0.6774(7) 0.93583(9) 0.6906(6) 0.0441(10) Uani 1 1 d . . . . .
H5A H 0.7231 0.9486 0.6041 0.053 Uiso 1 1 calc R . . . .
C5B C 1.1176(7) 0.56218(9) 0.6746(6) 0.0477(11) Uani 1 1 d . . . . .
H5B H 1.0998 0.5478 0.5761 0.057 Uiso 1 1 calc R . . . .
C6A C 0.6415(8) 0.94970(10) 0.8470(6) 0.0511(12) Uani 1 1 d . . . . .
C6B C 1.1599(7) 0.55015(9) 0.8475(6) 0.0425(10) Uani 1 1 d . . . . .
C7A C 0.5684(8) 0.93119(11) 0.9789(7) 0.0612(15) Uani 1 1 d . . . . .
H7A H 0.5426 0.9413 1.0843 0.073 Uiso 1 1 calc R . . . .
C7B C 1.1872(7) 0.57098(10) 0.9985(5) 0.0454(10) Uani 1 1 d . . . . .
H7B H 1.2166 0.5623 1.1152 0.054 Uiso 1 1 calc R . . . .
C8A C 0.5353(7) 0.89831(10) 0.9515(6) 0.0482(11) Uani 1 1 d . . . . .
H8A H 0.4878 0.8861 1.0390 0.058 Uiso 1 1 calc R . . . .
C8B C 1.1705(7) 0.60413(9) 0.9737(5) 0.0424(10) Uani 1 1 d . . . . .
H8B H 1.1879 0.6181 1.0741 0.051 Uiso 1 1 calc R . . . .
C9A C 0.5729(5) 0.88273(8) 0.7910(4) 0.0309(7) Uani 1 1 d . . . . .
C9B C 1.1269(5) 0.61756(8) 0.7963(4) 0.0264(7) Uani 1 1 d . . . . .
C10A C 0.5405(5) 0.84902(8) 0.7599(4) 0.0246(6) Uani 1 1 d . . . . .
H10A H 0.4912 0.8367 0.8458 0.030 Uiso 1 1 calc R . . . .
C10B C 1.1107(5) 0.65178(8) 0.7689(4) 0.0268(7) Uani 1 1 d . . . . .
H10B H 1.1291 0.6657 0.8695 0.032 Uiso 1 1 calc R . . . .
O3 O 1.2568(10) 0.49720(15) 1.2157(7) 0.122(2) Uani 1 1 d . . . C -1
H3C H 1.1720 0.4816 1.2529 0.36(10) Uiso 1 1 d G . . C -1
H3D H 1.3257 0.5051 1.3275 0.28(7) Uiso 1 1 d G . . C -1


_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
Co1 P1B 2.8040(8) 1_455 ?
Co1 O1 2.109(2) . ?
Co1 O2A 2.0513(19) . ?
Co1 O2B 2.2479(19) 1_455 ?
Co1 O2B 2.0716(18) 4_476 ?
Co1 O3A 2.0514(19) 4_576 ?
Co1 O3B 2.2027(19) 1_455 ?
Co2 P1A 2.7939(8) 4_575 ?
Co2 O2 2.108(2) . ?
Co2 O2A 2.2085(19) 4_575 ?
Co2 O3B 2.0666(19) 4_575 ?
Co2 O4A 2.2344(19) 4_575 ?
Co2 O4A 2.0591(18) . ?
Co2 O4B 2.0588(19) . ?
P1A Co2 2.7940(8) 4_576 ?
P1A O2A 1.5471(19) . ?
P1A O3A 1.5081(19) . ?
P1A O4A 1.548(2) . ?
P1A C1A 1.784(3) . ?
P1B Co1 2.8041(8) 1_655 ?
P1B O2B 1.548(2) . ?
P1B O3B 1.5485(19) . ?
P1B O4B 1.5081(19) . ?
P1B C1B 1.790(3) . ?
O1 H1A 0.9583 . ?
O1 H1B 0.9585 . ?
O1A H1AA 0.8200 . ?
O1A C6A 1.374(5) . ?
O1B H1BA 0.8200 . ?
O1B C6B 1.377(5) . ?
O2 H2A 0.9581 . ?
O2 H2B 0.9585 . ?
O2A Co2 2.2085(19) 4_576 ?
O2B Co1 2.2480(19) 1_655 ?
O2B Co1 2.0716(18) 4_675 ?
O3A Co1 2.0515(19) 4_575 ?
O3B Co1 2.2028(19) 1_655 ?
O3B Co2 2.0666(19) 4_576 ?
O4A Co2 2.2344(19) 4_576 ?
C1A C2A 1.420(4) . ?
C1A C10A 1.377(4) . ?
C1B C2B 1.416(4) . ?
C1B C10B 1.369(4) . ?
C2A H2AA 0.9300 . ?
C2A C3A 1.367(5) . ?
C2B H2BA 0.9300 . ?
C2B C3B 1.361(5) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.417(5) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.415(5) . ?
C4A C5A 1.426(5) . ?
C4A C9A 1.413(5) . ?
C4B C5B 1.417(5) . ?
C4B C9B 1.402(5) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.356(6) . ?
C5B H5B 0.9300 . ?
C5B C6B 1.365(5) . ?
C6A C7A 1.409(7) . ?
C6B C7B 1.396(6) . ?
C7A H7A 0.9300 . ?
C7A C8A 1.369(6) . ?
C7B H7B 0.9300 . ?
C7B C8B 1.365(5) . ?
C8A H8A 0.9300 . ?
C8A C9A 1.417(5) . ?
C8B H8B 0.9300 . ?
C8B C9B 1.417(5) . ?
C9A C10A 1.405(5) . ?
C9B C10B 1.410(4) . ?
C10A H10A 0.9300 . ?
C10B H10B 0.9300 . ?
O3 H3C 0.9590 . ?
O3 H3D 0.9580 . ?

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
O1 Co1 P1B 89.35(6) . 1_455 ?
O1 Co1 O2B 89.54(8) . 1_455 ?
O1 Co1 O3B 89.82(8) . 1_455 ?
O2A Co1 P1B 128.66(6) . 1_455 ?
O2A Co1 O1 91.71(8) . . ?
O2A Co1 O2B 100.21(8) . 4_476 ?
O2A Co1 O2B 95.24(7) . 1_455 ?
O2A Co1 O3B 161.96(7) . 1_455 ?
O2B Co1 P1B 131.06(6) 4_476 1_455 ?
O2B Co1 P1B 33.43(5) 1_455 1_455 ?
O2B Co1 O1 91.86(8) 4_476 . ?
O2B Co1 O2B 164.44(9) 4_476 1_455 ?
O2B Co1 O3B 97.70(7) 4_476 1_455 ?
O3A Co1 P1B 84.64(6) 4_576 1_455 ?
O3A Co1 O1 173.99(8) 4_576 . ?
O3A Co1 O2A 92.10(8) 4_576 . ?
O3A Co1 O2B 85.49(7) 4_576 1_455 ?
O3A Co1 O2B 92.03(8) 4_576 4_476 ?
O3A Co1 O3B 85.12(7) 4_576 1_455 ?
O3B Co1 P1B 33.37(5) 1_455 1_455 ?
O3B Co1 O2B 66.80(7) 1_455 1_455 ?
O2 Co2 P1A 90.27(6) . 4_575 ?
O2 Co2 O2A 90.30(8) . 4_575 ?
O2 Co2 O4A 89.79(7) . 4_575 ?
O2A Co2 P1A 33.51(5) 4_575 4_575 ?
O2A Co2 O4A 67.08(7) 4_575 4_575 ?
O3B Co2 P1A 129.03(6) 4_575 4_575 ?
O3B Co2 O2 90.91(8) 4_575 . ?
O3B Co2 O2A 162.51(7) 4_575 4_575 ?
O3B Co2 O4A 95.48(7) 4_575 4_575 ?
O4A Co2 P1A 129.99(6) . 4_575 ?
O4A Co2 P1A 33.57(5) 4_575 4_575 ?
O4A Co2 O2 92.71(8) . . ?
O4A Co2 O2A 96.54(7) . 4_575 ?
O4A Co2 O3B 100.84(8) . 4_575 ?
O4A Co2 O4A 163.45(8) . 4_575 ?
O4B Co2 P1A 84.14(6) . 4_575 ?
O4B Co2 O2 174.40(8) . . ?
O4B Co2 O2A 85.20(7) . 4_575 ?
O4B Co2 O3B 92.38(8) . 4_575 ?
O4B Co2 O4A 85.37(7) . 4_575 ?
O4B Co2 O4A 91.14(7) . . ?
O2A P1A Co2 52.00(7) . 4_576 ?
O2A P1A O4A 104.96(11) . . ?
O2A P1A C1A 108.58(12) . . ?
O3A P1A Co2 129.99(8) . 4_576 ?
O3A P1A O2A 113.19(11) . . ?
O3A P1A O4A 112.47(11) . . ?
O3A P1A C1A 109.07(12) . . ?
O4A P1A Co2 52.96(7) . 4_576 ?
O4A P1A C1A 108.36(12) . . ?
C1A P1A Co2 120.94(9) . 4_576 ?
O2B P1B Co1 53.15(7) . 1_655 ?
O2B P1B O3B 104.63(11) . . ?
O2B P1B C1B 110.05(12) . . ?
O3B P1B Co1 51.48(7) . 1_655 ?
O3B P1B C1B 108.56(12) . . ?
O4B P1B Co1 129.15(8) . 1_655 ?
O4B P1B O2B 112.51(11) . . ?
O4B P1B O3B 113.44(11) . . ?
O4B P1B C1B 107.59(12) . . ?
C1B P1B Co1 123.24(9) . 1_655 ?
Co1 O1 H1A 108.9 . . ?
Co1 O1 H1B 106.1 . . ?
H1A O1 H1B 104.4 . . ?
C6A O1A H1AA 109.5 . . ?
C6B O1B H1BA 109.5 . . ?
Co2 O2 H2A 110.5 . . ?
Co2 O2 H2B 108.3 . . ?
H2A O2 H2B 104.5 . . ?
Co1 O2A Co2 120.08(9) . 4_576 ?
P1A O2A Co1 124.14(11) . . ?
P1A O2A Co2 94.49(9) . 4_576 ?
Co1 O2B Co1 119.90(9) 4_675 1_655 ?
P1B O2B Co1 123.04(11) . 4_675 ?
P1B O2B Co1 93.42(9) . 1_655 ?
P1A O3A Co1 134.50(12) . 4_575 ?
Co2 O3B Co1 119.49(9) 4_576 1_655 ?
P1B O3B Co1 95.15(9) . 1_655 ?
P1B O3B Co2 123.27(11) . 4_576 ?
Co2 O4A Co2 121.34(9) . 4_576 ?
P1A O4A Co2 123.22(10) . . ?
P1A O4A Co2 93.47(9) . 4_576 ?
P1B O4B Co2 135.12(12) . . ?
C2A C1A P1A 119.8(2) . . ?
C10A C1A P1A 121.2(2) . . ?
C10A C1A C2A 119.0(3) . . ?
C2B C1B P1B 120.5(2) . . ?
C10B C1B P1B 121.1(2) . . ?
C10B C1B C2B 118.4(3) . . ?
C1A C2A H2AA 119.8 . . ?
C3A C2A C1A 120.5(3) . . ?
C3A C2A H2AA 119.8 . . ?
C1B C2B H2BA 119.6 . . ?
C3B C2B C1B 120.8(3) . . ?
C3B C2B H2BA 119.6 . . ?
C2A C3A H3A 119.5 . . ?
C2A C3A C4A 121.0(3) . . ?
C4A C3A H3A 119.5 . . ?
C2B C3B H3B 119.4 . . ?
C2B C3B C4B 121.3(3) . . ?
C4B C3B H3B 119.4 . . ?
C3A C4A C5A 122.0(3) . . ?
C9A C4A C3A 118.8(3) . . ?
C9A C4A C5A 119.2(3) . . ?
C3B C4B C5B 123.0(3) . . ?
C9B C4B C3B 118.3(3) . . ?
C9B C4B C5B 118.7(3) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A C4A 119.8(4) . . ?
C6A C5A H5A 120.1 . . ?
C4B C5B H5B 120.0 . . ?
C6B C5B C4B 120.0(4) . . ?
C6B C5B H5B 120.0 . . ?
O1A C6A C7A 115.4(4) . . ?
C5A C6A O1A 123.1(4) . . ?
C5A C6A C7A 121.5(4) . . ?
O1B C6B C7B 120.1(4) . . ?
C5B C6B O1B 118.3(4) . . ?
C5B C6B C7B 121.5(4) . . ?
C6A C7A H7A 120.1 . . ?
C8A C7A C6A 119.8(4) . . ?
C8A C7A H7A 120.1 . . ?
C6B C7B H7B 120.2 . . ?
C8B C7B C6B 119.5(4) . . ?
C8B C7B H7B 120.2 . . ?
C7A C8A H8A 119.7 . . ?
C7A C8A C9A 120.6(4) . . ?
C9A C8A H8A 119.7 . . ?
C7B C8B H8B 119.7 . . ?
C7B C8B C9B 120.6(4) . . ?
C9B C8B H8B 119.7 . . ?
C4A C9A C8A 119.1(3) . . ?
C10A C9A C4A 119.2(3) . . ?
C10A C9A C8A 121.7(3) . . ?
C4B C9B C8B 119.6(3) . . ?
C4B C9B C10B 119.3(3) . . ?
C10B C9B C8B 121.1(3) . . ?
C1A C10A C9A 121.6(3) . . ?
C1A C10A H10A 119.2 . . ?
C9A C10A H10A 119.2 . . ?
C1B C10B C9B 121.9(3) . . ?
C1B C10B H10B 119.0 . . ?
C9B C10B H10B 119.0 . . ?
H3C O3 H3D 104.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1A H1AA O1B 0.82 2.03 2.754(5) 147.4 2_756
O1B H1BA O3 0.82 1.85 2.662(6) 168.0 .

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.714
_oxdiff_exptl_absorpt_empirical_full_min 0.480
####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1956357'
loop_
_audit_author_name
_audit_author_address
Perez
;CRISMAT
France
;
_audit_update_record             
;
2019-09-27 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
'manganese 6-hydroxy-2-naphtylphosphonate hydrate'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C20 H18 Mn2 O11 P2'
_chemical_formula_weight         606.2
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ycb'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y+1/2,z+1/2

_cell_length_a                   7.4672(3)
_cell_length_b                   40.7737(9)
_cell_length_c                   7.6132(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.045(8)
_cell_angle_gamma                90
_cell_volume                     2289.1(3)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.998 1 0 0 0 1 0 0 0 1
2 0.002 0.0297 0 1.0143 0 -1 0 0.985 0 -0.0297

_cell_formula_units_Z            4

_cell_measurement_reflns_used    21445
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      39.18
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.7589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1228

_exptl_absorpt_coefficient_mu    1.303
_exptl_crystal_description       platelette
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            12166
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         39.53
_diffrn_reflns_theta_full        36.4
_diffrn_measured_fraction_theta_max 0.88
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             12166
_reflns_number_gt                4572
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1097
_refine_ls_wR_factor_gt          0.1031
_refine_ls_R_factor_all          0.2631
_refine_ls_wR_factor_ref         0.1256
_refine_ls_goodness_of_fit_ref   2.40
_refine_ls_goodness_of_fit_gt    3.26
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         12166
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_number_constraints    -41
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0868
_refine_ls_shift/su_mean         0.0136
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.3368 0.7283 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn -0.24133(9) -0.255254(18) 0.30411(11) Uani 0.0144(2) 4 1 d . . .
Mn2 Mn -0.74114(9) -0.244282(18) 0.30286(11) Uani 0.0141(2) 4 1 d . . .
P1 P 0.039772 -0.292592 0.082323 Uani 0.0119(4) 4 1 d . . .
P2 P -0.4572(3) -0.29193(6) 0.5847(4) Uani 0.0137(4) 4 1 d . . .
O1 O -0.4936(4) -0.22262(8) 0.2617(5) Uani 0.0180(11) 4 1 d . . .
O2 O -0.111962 -0.213828 0.433313 Uani 0.0192(11) 4 1 d . . .
O3 O -0.6116(4) -0.28602(8) 0.4307(5) Uani 0.0183(11) 4 1 d . . .
O4 O -0.39911(8) -0.29391(6) 0.1424(4) Uani 0.0217(12) 4 1 d . . .
O5 O -0.2772(4) -0.27793(8) 0.5473(5) Uiso 0.0163(7) 4 1 d . . .
O6 O 0.0059 -0.276844 0.258926 Uani 0.0121(10) 4 1 d . . .
O7 O -0.8982(9) -0.20507(17) 0.1467(9) Uani 0.0216(12) 4 1 d . . .
O8 O -0.779596 -0.223113 0.547272 Uani 0.0149(10) 4 1 d . . .
C9 C 0.075205 -0.335563 0.116309 Uani 0.0192(16) 4 1 d . . .
C10 C -0.4358(6) -0.33578(13) 0.6098(7) Uani 0.0198(15) 4 1 d . . .
O9 O -0.3146(10) -0.48360(11) 0.8749(8) Uani 0.106(4) 4 1 d . . .
O10 O 0.1694(12) -0.48316(14) 0.3850(12) Uani 0.136(5) 4 1 d . . .
C4 C -0.3926(8) -0.34962(13) 0.7711(9) Uani 0.034(2) 4 1 d . . .
C5 C 0.0370(7) -0.35023(13) 0.2668(8) Uani 0.0266(18) 4 1 d . . .
C6 C 0.1468(8) -0.35383(14) -0.0107(8) Uani 0.033(2) 4 1 d . . .
C7 C 0.1452(9) -0.40265(15) 0.1688(11) Uani 0.042(3) 4 1 d . . .
C8 C -0.4003(10) -0.40388(15) 0.6537(11) Uani 0.047(3) 4 1 d . . .
C11 C -0.4612(10) -0.35674(16) 0.4649(10) Uani 0.053(3) 4 1 d . . .
C12 C 0.0711(10) -0.38398(14) 0.2970(10) Uani 0.040(2) 4 1 d . . .
C13 C -0.3732(8) -0.38361(15) 0.7992(10) Uani 0.035(2) 4 1 d . . .
C14 C -0.3386(12) -0.45099(17) 0.8508(14) Uani 0.067(4) 4 1 d . . .
C15 C -0.4450(13) -0.39012(16) 0.4855(11) Uani 0.073(4) 4 1 d . . .
C16 C 0.1751(11) -0.43689(17) 0.1973(15) Uani 0.069(4) 4 1 d . . .
C17 C 0.1823(9) -0.38657(14) 0.0161(10) Uani 0.043(2) 4 1 d . . .
C18 C -0.3828(11) -0.43869(16) 0.6789(12) Uani 0.062(3) 4 1 d . . .
C19 C -0.3126(12) -0.42990(17) 0.9977(13) Uani 0.071(4) 4 1 d . . .
C20 C 0.0354(13) -0.40002(17) 0.4515(13) Uani 0.080(4) 4 1 d . . .
C21 C -0.3315(12) -0.39689(17) 0.9699(12) Uani 0.068(3) 4 1 d . . .
C22 C 0.1394(15) -0.45073(20) 0.3501(16) Uani 0.088(5) 4 1 d . . .
C1 C 0.0668(15) -0.4326(2) 0.4782(15) Uani 0.102(5) 4 1 d . . .
O11 O -0.241(2) -0.5027(3) 1.2171(11) Uani 0.209(8) 4 1 d . . .
H2o4 H -0.534078 -0.294659 0.13367 Uiso 0.040(18) 4 1 d . . .
H1o7 H -0.876(8) -0.2021(15) 0.060(8) Uiso 0.013(17) 4 1 d . . .
H1c4 H -0.373774 -0.335476 0.873115 Uiso 0.0407 4 1 d . . .
H1c5 H -0.013685 -0.33751 0.353067 Uiso 0.0319 4 1 d . . .
H1c6 H 0.171404 -0.343436 -0.117579 Uiso 0.04 4 1 d . . .
H1c11 H -0.490725 -0.347729 0.347424 Uiso 0.0632 4 1 d . . .
H1c15 H -0.464831 -0.40408 0.382757 Uiso 0.0881 4 1 d . . .
H1c16 H 0.220146 -0.450046 0.109243 Uiso 0.0824 4 1 d . . .
H1c17 H 0.233758 -0.398747 -0.071681 Uiso 0.0518 4 1 d . . .
H1c18 H -0.401196 -0.453264 0.578665 Uiso 0.0749 4 1 d . . .
H1c19 H -0.281956 -0.438493 1.116021 Uiso 0.0852 4 1 d . . .
H1c20 H -0.01254 -0.387581 0.540554 Uiso 0.0958 4 1 d . . .
H1c21 H -0.315723 -0.382402 1.070531 Uiso 0.0811 4 1 d . . .
H1c1 H 0.0395 -0.443119 0.583774 Uiso 0.122 4 1 d . . .
H1o10 H 0.233345 -0.497147 0.348531 Uiso 0.1634 4 1 d . . .
H1o9 H -0.354397 -0.497586 0.93591 Uiso 0.1275 4 1 d . . .
H1o11 H -0.283421 -0.519885 1.248465 Uiso 0.2508 4 1 d . . .
H2o11 H -0.176923 -0.491245 1.290083 Uiso 0.2508 4 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
P1 P -0.0142(9) -0.00153(10) -0.0041(6) -0.00005(2) 0.00041(8) -0.0010(6)
-0.000084(8) -0.00025(3) -0.00184(12) -0.0130(9)
P2 P 0.0171(10) 0.00186(11) 0.0063(6) 0.00004(2) -0.00007(9) 0.0027(7)
0.000061(8) 0.00034(3) 0.00279(16) 0.0185(13)
O7 O 0.000(4) -0.0001(4) -0.006(2) -0.00001(7) -0.0005(3) 0.000(2) -0.00003(2)
-0.00015(8) -0.0002(4) 0.003(3)

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O2 . . 2.1107 ?
Mn1 O5 . . 2.124(4) ?
Mn1 O6 . . 2.1216 ?
Mn2 O1 . . 2.116(3) ?
Mn2 O3 . . 2.117(3) ?
Mn2 O8 . . 2.1114 ?
P1 O2 . 4_544 1.495 ?
P1 O6 . . 1.5463 ?
P1 O8 . 4_644 1.5536 ?
P1 C9 . . 1.7847 ?
P2 O1 . 4_545 1.535(5) ?
P2 O3 . . 1.529(4) ?
P2 O5 . . 1.528(4) ?
P2 C10 . . 1.802(6) ?
O7 H1o7 . . 0.71(6) ?
C9 C5 . . 1.3618 ?
C9 C6 . . 1.3924 ?
C10 C4 . . 1.343(8) ?
C10 C11 . . 1.385(9) ?
O9 C14 . . 1.350(9) ?
O9 H1o9 . . 0.82 ?
O10 C22 . . 1.360(10) ?
O10 H1o10 . . 0.82 ?
C4 C13 . . 1.406(8) ?
C4 H1c4 . . 0.96 ?
C5 C12 . . 1.412(8) ?
C5 H1c5 . . 0.96 ?
C6 C17 . . 1.370(8) ?
C6 H1c6 . . 0.96 ?
C7 C12 . . 1.417(11) ?
C7 C16 . . 1.425(9) ?
C7 C17 . . 1.399(11) ?
C8 C13 . . 1.371(10) ?
C8 C15 . . 1.390(11) ?
C8 C18 . . 1.435(9) ?
C11 C15 . . 1.373(9) ?
C11 H1c11 . . 0.96 ?
C12 C20 . . 1.407(12) ?
C13 C21 . . 1.397(11) ?
C14 C18 . . 1.392(13) ?
C14 C19 . . 1.400(13) ?
C15 H1c15 . . 0.96 ?
C16 C22 . . 1.356(16) ?
C16 H1c16 . . 0.96 ?
C17 H1c17 . . 0.96 ?
C18 H1c18 . . 0.96 ?
C19 C21 . . 1.367(10) ?
C19 H1c19 . . 0.96 ?
C20 C1 . . 1.360(11) ?
C20 H1c20 . . 0.96 ?
C21 H1c21 . . 0.96 ?
C22 C1 . . 1.398(16) ?
C1 H1c1 . . 0.96 ?
O11 H1o11 . . 0.82 ?
O11 H2o11 . . 0.82 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Mn1 O5 . . . 93.05 ?
O2 Mn1 O6 . . . 93.52 ?
O5 Mn1 O6 . . . 101.12 ?
O1 Mn2 O3 . . . 93.27(13) ?
O1 Mn2 O8 . . . 101.7 ?
O3 Mn2 O8 . . . 92.23 ?
O2 P1 O6 4_544 . . 112.27 ?
O2 P1 O8 4_544 . 4_644 111.86 ?
O2 P1 C9 4_544 . . 111.06 ?
O6 P1 O8 . . 4_644 104.08 ?
O6 P1 C9 . . . 108.81 ?
O8 P1 C9 4_644 . . 108.46 ?
O1 P2 O3 4_545 . . 113.3(2) ?
O1 P2 O5 4_545 . . 107.5(2) ?
O1 P2 C10 4_545 . . 108.4(3) ?
O3 P2 O5 . . . 112.2(2) ?
O3 P2 C10 . . . 106.3(2) ?
O5 P2 C10 . . . 108.9(2) ?
Mn2 O1 P2 . . 4_544 124.8(2) ?
Mn1 O2 P1 . . 4_545 136.93 ?
Mn2 O3 P2 . . . 135.6(2) ?
Mn1 O5 P2 . . . 124.1(2) ?
Mn1 O6 P1 . . . 125.36 ?
Mn2 O8 P1 . . 4_445 124.19 ?
P1 C9 C5 . . . 120.47 ?
P1 C9 C6 . . . 119.25 ?
C5 C9 C6 . . . 120.25 ?
P2 C10 C4 . . . 121.2(4) ?
P2 C10 C11 . . . 121.9(4) ?
C4 C10 C11 . . . 116.9(5) ?
C14 O9 H1o9 . . . 135.24 ?
C22 O10 H1o10 . . . 134.15 ?
C10 C4 C13 . . . 123.9(6) ?
C10 C4 H1c4 . . . 118.07 ?
C13 C4 H1c4 . . . 118.07 ?
C9 C5 C12 . . . 120.57 ?
C9 C5 H1c5 . . . 119.71 ?
C12 C5 H1c5 . . . 119.71 ?
C9 C6 C17 . . . 120.25 ?
C9 C6 H1c6 . . . 119.87 ?
C17 C6 H1c6 . . . 119.88 ?
C12 C7 C16 . . . 119.3(8) ?
C12 C7 C17 . . . 118.0(6) ?
C16 C7 C17 . . . 122.6(8) ?
C13 C8 C15 . . . 119.0(6) ?
C13 C8 C18 . . . 119.3(7) ?
C15 C8 C18 . . . 121.7(7) ?
C10 C11 C15 . . . 121.5(7) ?
C10 C11 H1c11 . . . 119.26 ?
C15 C11 H1c11 . . . 119.27 ?
C5 C12 C7 . . . 119.4(7) ?
C5 C12 C20 . . . 122.4(7) ?
C7 C12 C20 . . . 118.1(6) ?
C4 C13 C8 . . . 118.2(6) ?
C4 C13 C21 . . . 121.7(6) ?
C8 C13 C21 . . . 120.0(6) ?
O9 C14 C18 . . . 119.3(8) ?
O9 C14 C19 . . . 119.8(8) ?
C18 C14 C19 . . . 120.8(7) ?
C8 C15 C11 . . . 120.6(7) ?
C8 C15 H1c15 . . . 119.69 ?
C11 C15 H1c15 . . . 119.69 ?
C7 C16 C22 . . . 119.4(9) ?
C7 C16 H1c16 . . . 120.29 ?
C22 C16 H1c16 . . . 120.29 ?
C6 C17 C7 . . . 121.4(7) ?
C6 C17 H1c17 . . . 119.28 ?
C7 C17 H1c17 . . . 119.28 ?
C8 C18 C14 . . . 119.0(7) ?
C8 C18 H1c18 . . . 120.49 ?
C14 C18 H1c18 . . . 120.49 ?
C14 C19 C21 . . . 118.9(8) ?
C14 C19 H1c19 . . . 120.55 ?
C21 C19 H1c19 . . . 120.56 ?
C12 C20 C1 . . . 121.9(9) ?
C12 C20 H1c20 . . . 119.05 ?
C1 C20 H1c20 . . . 119.05 ?
C13 C21 C19 . . . 121.9(8) ?
C13 C21 H1c21 . . . 119.05 ?
C19 C21 H1c21 . . . 119.05 ?
O10 C22 C16 . . . 121.6(10) ?
O10 C22 C1 . . . 116.5(10) ?
C16 C22 C1 . . . 121.9(8) ?
C20 C1 C22 . . . 119.2(10) ?
C20 C1 H1c1 . . . 120.39 ?
C22 C1 H1c1 . . . 120.39 ?
H1o11 O11 H2o11 . . . 120 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H2o4 O3 . . . 1.00 2.45 2.922(5) 108.46 ?
O4 H2o4 O8 . . 4_544 1.00 1.98 2.9037 151.59 ?
O7 H1o7 O3 . . 4_544 0.71(6) 2.39(6) 2.919(8) 132(6) ?
O7 H1o7 O6 . . 4_444 0.71(6) 2.48 3.0182 130(60) ?
O10 H1o10 O9 . . 3_546 0.82 2.05 2.758(11) 144.27 ?
O9 H1o9 O11 . . . 0.82 2.18 2.691(10) 120.15 ?


