Crystal structure of catena-poly[diaqua-(μ2-2,5-dihydroxyterephthalato-κ4 O,O′:O′′,O′′′)cadmium(II)], C8H8O8Cd
Xue, Li-ping; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 271–272; doi:10.1515/ncrs-2017-0270

data_8106122
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-(\m2-2,5-dihydroxyterephthalato-\k4
 O,O&#x2032;:O&#x2032;&#x2032;,O&#x2032;&#x2032;&#x2032;)cadmium(II)],
 C8H8O8Cd
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              271
_journal_page_last               272
_journal_paper_doi               10.1515/ncrs-2017-0270
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         '0.5(C16 H16 Cd2 O16)'
_chemical_formula_sum            'C8 H8 Cd O8'
_chemical_formula_weight         344.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 108.992(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5170(11)
_cell_length_b                   5.4639(3)
_cell_length_c                   11.5875(9)
_cell_measurement_reflns_used    2290
_cell_measurement_temperature    286.74(11)
_cell_measurement_theta_max      27.2350
_cell_measurement_theta_min      4.5390
_cell_volume                     988.81(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      286.74(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_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    -20.00  26.00   1.00    5.00    --  -12.53 -99.00  30.00   46
  2  \w     34.00  86.00   1.00    5.00    --   13.55-178.00  30.00   52
  3  \w    -13.00  81.00   1.00    5.00    --   13.55  77.00  90.00   94
  4  \w     34.00  86.00   1.00    5.00    --   13.55-178.00 -90.00   52
  5  \w    -46.00   8.00   1.00    5.00    --  -12.53  90.00  34.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0181106000
_diffrn_orient_matrix_UB_12      -0.1093482000
_diffrn_orient_matrix_UB_13      -0.0138462000
_diffrn_orient_matrix_UB_21      -0.0050554000
_diffrn_orient_matrix_UB_22      0.0452476000
_diffrn_orient_matrix_UB_23      -0.0592986000
_diffrn_orient_matrix_UB_31      0.0413575000
_diffrn_orient_matrix_UB_32      0.0532958000
_diffrn_orient_matrix_UB_33      0.0219154000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2735
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.482
_diffrn_reflns_theta_min         3.719
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                870
_reflns_number_total             908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0270_suppl.cif
_cod_data_source_block           46b33
_cod_database_code               8106122
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.544
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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:
 O3(H1W,H2W)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              60067
_shelx_hkl_checksum              26151
_olex2_date_sample_data_collection 2017-04-11
_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 1.434
_oxdiff_exptl_absorpt_empirical_full_min 0.826