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_7703013
_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 Cu2 O10 P2, 0.5(H4 O2)'
_chemical_formula_sum            'C20 H20 Cu2 O11 P2'
_chemical_formula_weight         625.38
_chemical_name_systematic
'copper 6-hydroxy-2-naphtylphosphonate hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-27 deposited with the CCDC.	2019-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0499(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.66017(4)
_cell_length_b                   4.75153(4)
_cell_length_c                   41.0950(3)
_cell_measurement_reflns_used    18919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.4440
_cell_measurement_theta_min      4.2850
_cell_volume                     1103.663(15)
_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)'
_diffrn_ambient_temperature      293
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     18.00 114.00   0.40   30.00    --   43.75  19.00  60.00  240
  2  \w     65.00  91.00   0.40   30.00    --   43.75  77.00 -30.00   65
  3  \w    105.00 130.20   0.40   30.00    --  110.00 137.00 -51.00   63
  4  \w    113.00 152.20   0.40   30.00    --  110.00 125.00 -60.00   98
  5  \w    134.00 160.00   0.40   30.00    --  110.00 125.00 -90.00   65
  6  \w    120.00 167.20   0.40   30.00    --  110.00  77.00 -30.00  118
  7  \w    127.00 153.00   0.40   30.00    --  110.00  15.00 -90.00   65
  8  \w    120.00 145.20   0.40   30.00    --  110.00  45.00 -30.00   63
  9  \w    113.00 139.00   0.40   30.00    --  110.00 -15.00   0.00   65
 10  \w    111.00 137.00   0.40   30.00    --  110.00 -15.00  60.00   65
 11  \w     96.00 122.00   0.40   30.00    --  110.00 -45.00 120.00   65
 12  \w     93.00 129.00   0.40   30.00    --  110.00 -61.00  90.00   90
 13  \w     86.00 112.00   0.40   30.00    --  110.00 -45.00  30.00   65
 14  \w     64.00  98.00   0.40   30.00    --  110.00 -94.00  90.00   85
 15  \w     55.00  80.20   0.40   30.00    --  110.00-132.00  62.00   63
 16  \w     59.00  96.20   0.40   30.00    --  110.00 -94.00  60.00   93
 17  \w     57.00  82.20   0.40   30.00    --  110.00 -45.00 120.00   63
 18  \w     51.00  80.20   0.40   30.00    --  110.00 -45.00  30.00   73
 19  \w     59.00  90.20   0.40   30.00    --  110.00 -15.00   0.00   78
 20  \w     59.00  85.00   0.40   30.00    --  110.00 -30.00 -60.00   65
 21  \w     98.00 130.00   0.40   30.00    --  110.00 -61.00-120.00   80
 22  \w     79.00 110.20   0.40   30.00    --  110.00-125.00-180.00   78
 23  \w     69.00  94.20   0.40   30.00    --  110.00-137.00-114.00   63
 24  \w     71.00 103.00   0.40   30.00    --  110.00-125.00 -90.00   80
 25  \w     68.00 133.20   0.40   30.00    --  110.00 -77.00-120.00  163
 26  \w     77.00 127.00   0.40   30.00    --  110.00 -30.00-120.00  125
 27  \w    127.00 153.00   0.40   30.00    --  110.00  15.00-180.00   65
 28  \w     99.00 131.00   0.40   30.00    --  110.00  45.00-120.00   80
 29  \w     97.00 170.20   0.40   30.00    --  110.00  45.00 -60.00  183
 30  \w    104.00 170.00   0.40   30.00    --  110.00  61.00  30.00  165
 31  \w    110.00 147.20   0.40   30.00    --  110.00  30.00  60.00   93
 32  \w     82.00 113.20   0.40   30.00    --  110.00  77.00 -60.00   78
 33  \w     86.00 168.00   0.40   30.00    --  110.00  77.00-120.00  205
 34  \w    105.00 156.20   0.40   30.00    --  110.00 125.00-180.00  128
 35  \w     94.00 162.00   0.40   30.00    --  110.00 125.00-120.00  170
 36  \w     91.00 147.00   0.40   30.00    --  110.00 132.00 131.00  140
 37  \w     16.00 107.20   0.40   30.00    --   43.75  77.00 -90.00  228
 38  \w     35.00  64.20   0.40   30.00    --  110.00 -30.00-120.00   73
 39  \w     66.00 122.00   0.40   30.00    --  110.00 -45.00-150.00  140
 40  \w     73.00 132.20   0.40   30.00    --  110.00 -77.00-180.00  148
 41  \w     73.00 116.20   0.40   30.00    --  110.00 -61.00-150.00  108
 42  \w     49.00  86.20   0.40   30.00    --  110.00-125.00-150.00   93
 43  \w     43.00  71.00   0.40   30.00    --  110.00-125.00-180.00   70
 44  \w     39.00  66.20   0.40   30.00    --  110.00-125.00 -90.00   68
 45  \w     48.00  73.20   0.40   30.00    --  110.00 -45.00 -60.00   63
 46  \w     44.00 113.20   0.40   30.00    --  110.00 -61.00   0.00  173
 47  \w     58.00  89.20   0.40   30.00    --  110.00-125.00  90.00   78
 48  \w     43.00  88.20   0.40   30.00    --   43.75-132.00  62.00  113
 49  \w     13.00  54.20   0.40   30.00    --   43.75 -38.00  90.00  103
 50  \w    -27.00   5.00   0.40   30.00    --   43.75 -38.00  90.00   80
 51  \w     16.00  43.20   0.40   30.00    --   43.75  77.00 -30.00   68
 52  \w     32.00  65.20   0.40   30.00    --   43.75 -77.00-180.00   83
 53  \w     43.00  72.20   0.40   30.00    --   43.75-137.00-114.00   73
 54  \w     -2.00  29.20   0.40   30.00    --   -0.75 -94.00-120.00   78
 55  \w      6.00  33.20   0.40   30.00    --   -0.75 -94.00-180.00   68
 56  \w    -21.00  19.00   0.40   30.00    --   43.75 -77.00-180.00  100
 57  \w    112.00 138.00   0.40   30.00    --  110.00 132.00 131.00   65
 58  \w     15.00  49.00   0.40   30.00    --   43.75  77.00 150.00   85
 59  \w     27.00  53.00   0.40   30.00    --   43.75 -99.00   0.00   65
 60  \w     16.00  66.00   0.40   30.00    --   43.75  77.00 -60.00  125
 61  \w     69.00  98.20   0.40   30.00    --   43.75  77.00 150.00   73
 62  \w     65.00 103.00   0.40   30.00    --   43.75  77.00  30.00   95
 63  \w     82.00 107.20   0.40   30.00    --   43.75  77.00-150.00   63
 64  \w     16.00  50.00   0.40   30.00    --   43.75  77.00-180.00   85
 65  \w     15.00  65.00   0.40   30.00    --   43.75  77.00-150.00  125
 66  \w    -20.00  15.20   0.40   30.00    --   43.75 -77.00 -60.00   88
 67  \w      0.00  53.20   0.40   30.00    --   43.75 -99.00  60.00  133
 68  \w     17.00  55.00   0.40   30.00    --   43.75  77.00  30.00   95
 69  \w     15.00  60.20   0.40   30.00    --   43.75  77.00  90.00  113
 70  \w     17.00  60.20   0.40   30.00    --   43.75  77.00   0.00  108
 71  \w     27.00  61.00   0.40   30.00    --   43.75 -77.00 -60.00   85
 72  \w     71.00 107.00   0.40   30.00    --   43.75  77.00  90.00   90
 73  \w     64.00 105.20   0.40   30.00    --   43.75  77.00-180.00  103
 74  \w     81.00 107.00   0.40   30.00    --  110.00  77.00 -90.00   65
 75  \w     81.00 145.00   0.40   30.00    --  110.00  77.00  90.00  160
 76  \w    131.00 171.00   0.40   30.00    --  110.00  61.00  60.00  100
 77  \w     81.00 106.20   0.40   30.00    --  110.00  77.00-150.00   63
 78  \w     85.00 111.00   0.40   30.00    --  110.00  77.00 -54.17   65
 79  \w    143.80 171.00   0.40   30.00    --  110.00  77.00  30.00   68
 80  \w     89.00 126.20   0.40   30.00    --  110.00  61.00  60.00   93
 81  \w     81.00 122.20   0.40   30.00    --  110.00  78.00 106.13  103
 82  \w    132.00 159.20   0.40   30.00    --  110.00  78.00 106.13   68
 83  \w     84.00 109.20   0.40   30.00    --  110.00  71.00   1.64   63
 84  \w     48.00  87.20   0.40   30.00    --  110.00 -45.00-180.00   98
 85  \w     81.00 120.20   0.40   30.00    --  110.00  78.00 171.77   98
 86  \w    141.00 167.00   0.40   30.00    --  110.00  78.00 171.77   65
 87  \w    139.00 170.20   0.40   30.00    --  110.00  72.00  19.22   78
 88  \w     83.00 109.00   0.40   30.00    --  110.00  72.00  19.22   65
 89  \w     81.00 107.00   0.40   30.00    --  110.00  77.00  30.00   65
 90  \w     89.00 115.00   0.40   30.00    --  110.00  61.00-150.00   65
 91  \w    145.00 170.20   0.40   30.00    --  110.00  30.00   0.00   63
 92  \w     80.00 106.00   0.40   30.00    --  110.00  80.00 -28.21   65
 93  \w     81.00 149.00   0.40   30.00    --  110.00  77.00 120.00  170
 94  \w     95.00 126.20   0.40   30.00    --  110.00  30.00   0.00   78
 95  \w    140.00 167.20   0.40   30.00    --  110.00  61.00  90.00   68
 96  \w     89.00 115.00   0.40   30.00    --  110.00  61.00  90.00   65
 97  \w     89.00 114.20   0.40   30.00    --  110.00  61.00 -90.00   63
 98  \w     81.00 125.00   0.40   30.00    --  110.00  77.00 140.28  110
 99  \w     81.00 107.00   0.40   30.00    --  110.00  77.00-120.00   65
100  \w     89.00 115.00   0.40   30.00    --  110.00  61.00   0.00   65
101  \w     89.00 114.20   0.40   30.00    --  110.00  61.00-180.00   63
102  \w    125.00 166.20   0.40   30.00    --  110.00  61.00-180.00  103
103  \w     83.00 113.00   0.40   30.00    --  110.00  74.00-143.23   75
104  \w     81.00 106.20   0.40   30.00    --  110.00  77.00 -30.00   63
105  \w    134.00 160.00   0.40   30.00    --  110.00  77.00 -30.00   65
106  \w     99.00 151.00   0.40   30.00    --  110.00  45.00-150.00  130
107  \w     94.00 120.00   0.40   30.00    --  110.00  30.00 -30.00   65
108  \w    139.00 165.00   0.40   30.00    --  110.00  61.00 -60.00   65
109  \w     82.00 132.00   0.40   30.00    --  110.00  77.00 154.12  125
110  \w     81.00 146.20   0.40   30.00    --  110.00  77.00  60.00  163
111  \w     89.00 114.20   0.40   30.00    --  110.00  61.00 -60.00   63
112  \w     82.00 108.00   0.40   30.00    --  110.00  77.00-180.00   65
113  \w    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       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_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
_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_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.882
_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
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0374
_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/[\s^2^(Fo^2^)+(0.0224P)^2^+3.8156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2269
_reflns_number_total             2278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03947c2.cif
_cod_data_source_block           fb144ht_cr1
_cod_depositor_comments
'Adding full bibliography for 7703013--7703015.cif.'
_cod_original_cell_volume        1103.662(14)
_cod_database_code               7703013
_shelx_shelxl_version_number     2017/1
_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)
;
_shelx_res_checksum              55164
_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
;