The crystal structure of catena-poly[aqua-2,2′bipyridine-κ2 N,N′-(μ2-5-ethoxyisophthalato-κ 4 O,O′:Oʺ,O′ʺ)cadmium(II)] monohydrate, C20H20CdN2O7
Zhang, Lilei; Chang, Deming; Dun, Mengdan; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 615–617; doi:10.1515/ncrs-2022-0057

data_8107169
_publ_section_title
;
 The crystal structure of catena-poly[aqua-2,2&#x2032;bipyridine-\k2
 N,N&#x2032;-(\m2-5-ethoxyisophthalato-\k 4
 O,O&#x2032;:O&#x02BA;,O&#x2032;&#x02BA;)cadmium(II)] monohydrate,
 C20H20CdN2O7
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              615
_journal_page_last               617
_journal_paper_doi               10.1515/ncrs-2022-0057
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C20 H18 Cd N2 O6, H2 O'
_chemical_formula_sum            'C20 H20 Cd N2 O7'
_chemical_formula_weight         512.78
_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     iterative
_cell_angle_alpha                90
_cell_angle_beta                 98.537(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0154(3)
_cell_length_b                   17.7168(8)
_cell_length_c                   12.8449(5)
_cell_measurement_reflns_used    4203
_cell_measurement_temperature    288.32(10)
_cell_measurement_theta_max      27.1400
_cell_measurement_theta_min      4.1390
_cell_volume                     2028.91(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r  [1]'
_computing_data_collection       'CrysAlisPro 1.171.38.41r  [1]'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r  [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015) [3]'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015) [3]'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      288.32(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     10.00  52.00   1.00    6.71    --  -12.53   0.00  60.00   42
  2  \w     17.00  50.00   1.00    6.71    --   13.55 -99.00 -30.00   33
  3  \w     10.00  76.00   1.00    6.71    --   13.55  57.00 -90.00   66
  4  \w    -74.00 -11.00   1.00    6.71    --  -12.53   0.00  60.00   63
;
_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      0.0768256000
_diffrn_orient_matrix_UB_12      -0.0097533000
_diffrn_orient_matrix_UB_13      0.0022033000
_diffrn_orient_matrix_UB_21      0.0164886000
_diffrn_orient_matrix_UB_22      0.0376894000
_diffrn_orient_matrix_UB_23      -0.0128022000
_diffrn_orient_matrix_UB_31      0.0130632000
_diffrn_orient_matrix_UB_32      0.0092189000
_diffrn_orient_matrix_UB_33      0.0542922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8050
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86915
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3139
_reflns_number_total             3545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0057_suppl.cif
_cod_data_source_block           281
_cod_database_code               8107169
_chemical_oxdiff_formula         'C H O N Cd'
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O6(H6a,H6b)
2.b Free rotating group:
 O7(H7c,H7d)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20)
2.e Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c)
;
_shelx_res_checksum              81181
_shelx_hkl_checksum              61139
_olex2_date_sample_data_collection 2016-12-18
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.816