M(H<sub>2</sub>O)(PO<sub>3</sub>C<sub>10</sub>H<sub>6</sub>OH)·(H<sub>2</sub>O)<sub>0.5</sub> (M = Co, Mn, Zn, Cu): a new series of layered metallophosphonate compounds obtained from 6-hydroxy-2-naphthylphosphonic acid.
Beaubras, Félicien; Rueff, Jean-Michel; Perez, Olivier; Veillon, Fabien; Caignaert, Vincent; Lohier, Jean-François; Cardin, Julien; Rogez, Guillaume; Jestin, Charlotte; Couthon, Hélène; Jaffrès, Paul-Alain; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3877–3891; doi:10.1039/c9dt03947c

data_7703014
_publ_section_title
;
 M(H<sub>2</sub>O)(PO<sub>3</sub>C<sub>10</sub>H<sub>6</sub>OH)&#x00B7;(H<sub>2</sub>O)<sub>0.5</sub>
 (M = Co, Mn, Zn, Cu): a new series of layered metallophosphonate
 compounds obtained from 6-hydroxy-2-naphthylphosphonic acid.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3877
_journal_page_last               3891
_journal_paper_doi               10.1039/c9dt03947c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H18 Co2 O10 P2, H2 O'
_chemical_formula_sum            'C20 H20 Co2 O11 P2'
_chemical_formula_weight         616.16
_chemical_name_systematic
'cobalt 6-hydroxy-2-naphtylphosphonate hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-09-27 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.144(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3353(3)
_cell_length_b                   40.691(2)
_cell_length_c                   7.4400(2)
_cell_measurement_reflns_used    12079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.9520
_cell_measurement_theta_min      2.9260
_cell_volume                     2192.48(15)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     39.33 140.83   0.50   40.00    --   35.00 175.00  30.00  203
  2  \f   -360.00   9.00   0.50   40.00 -38.81 -25.00 175.00    --   738
  3  \w     39.69 100.69   0.50   40.00    --   40.00 175.00 120.00  122
  4  \w     39.33 140.83   0.50   40.00    --   35.00 175.00 -25.00  203
  5  \w     39.63 134.63   0.50   40.00    --   40.00 175.00 -60.00  190
  6  \w     39.75 121.25   0.50   40.00    --   40.00 175.00 150.00  163
  7  \w     39.33 130.83   0.50   40.00    --   25.00 175.00-170.00  183
  8  \w     98.33 145.83   0.50   40.00    --   40.00 175.00  50.00   95
  9  \w     39.39  74.39   0.50   40.00    --   35.00 175.00 -45.00   70
 10  \w     54.79  87.79   0.50   40.00    --   40.00 175.00 -65.00   66
 11  \w     39.52 106.02   0.50   40.00    --   30.00 175.00  60.00  133
 12  \f   -360.00   9.00   0.50   40.00 -38.98  20.00 175.00    --   738
;
_diffrn_measurement_device_type  'Bruker Nonius four-circle  diffractometer'
_diffrn_measurement_method       '\w and \f 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_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source_current           600\mA
_diffrn_source_power             30W
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50kV
_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_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_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.101
_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_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0448
_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/[\s^2^(Fo^2^)+(0.0272P)^2^+7.4628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4717
_reflns_number_total             7693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03947c2.cif
_cod_data_source_block           fb316cristal2_col
_cod_depositor_comments
'Adding full bibliography for 7703013--7703015.cif.'
_cod_original_cell_volume        2192.50(16)
_cod_database_code               7703014
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Co1 P1 C10 O4 H11'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.782
_reflns_odcompleteness_completeness 84.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.06
_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)
;
_shelx_res_checksum              7179
_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