Crystal structure of poly[diaqua-(μ4-4-(3,5-dicarboxy-κ1O-phenoxy)phthalato-κ3O:O′:O′)cadmium(II)], C16H12CdO11
Sun, Tao; Li, Ke; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1283–1284; doi:10.1515/ncrs-2019-0407

data_8106007
_publ_section_title
;
 Crystal structure of
 poly[diaqua-(\m4-4-(3,5-dicarboxy-\k1O-phenoxy)phthalato-\k3O:O&#x2032;:O&#x2032;)cadmium(II)],
 C16H12CdO11
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1283
_journal_page_last               1284
_journal_paper_doi               10.1515/ncrs-2019-0407
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C16 H12 Cd O11'
_chemical_formula_sum            'C16 H12 Cd O11'
_chemical_formula_weight         492.66
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.802(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6977(6)
_cell_length_b                   5.9706(2)
_cell_length_c                   20.7220(10)
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2280
_cell_measurement_theta_min      3.9740
_cell_volume                     1710.91(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_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    -41.00  54.00   1.00   20.00    --  -13.80  77.00 -60.00   95
  2  \w    -20.00  25.00   1.00   20.00    --  -13.80 -99.00   0.00   45
  3  \w    -20.00  25.00   1.00   20.00    --  -13.80 -99.00-180.00   45
  4  \w    -20.00  54.00   1.00   20.00    --   14.82 -99.00  30.00   74
  5  \w     -2.00  82.00   1.00   20.00    --   14.82  57.00-120.00   84
  6  \w     -4.00  84.00   1.00   20.00    --   14.82  38.00-150.00   88
  7  \w    -57.00  44.00   1.00   20.00    --   14.82 -19.00  30.00  101
  8  \w    -86.00 -61.00   1.00   20.00    --  -13.80-178.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356962000
_diffrn_orient_matrix_UB_12      0.0129013000
_diffrn_orient_matrix_UB_13      0.0157686000
_diffrn_orient_matrix_UB_21      -0.0359195000
_diffrn_orient_matrix_UB_22      0.0139670000
_diffrn_orient_matrix_UB_23      -0.0327131000
_diffrn_orient_matrix_UB_31      -0.0082320000
_diffrn_orient_matrix_UB_32      -0.1171832000
_diffrn_orient_matrix_UB_33      -0.0021759000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18198
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.966
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                2916
_reflns_number_total             3178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2019-0407_suppl.cif
_cod_data_source_block           s3
_cod_database_code               8106007
_chemical_oxdiff_formula         'C H N O CD'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14)
2.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O11(H11)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.377
_oxdiff_exptl_absorpt_empirical_full_min 0.469