Crystal structure of catena-poly[tetraaqua-(μ2-4,4′-bipyridine-k2 N:N′)-bis(μ2-4′-methyl-[1,1′-biphenyl]-3,5-dicarboxylato-k4 O,O′:O″,O′″)dicadmium(II)] dihydrate, C20H20NO7Cd
Chen, Shi-Jun; Cao, Xin; Ma, Xin-Dong; Xi, Zhong-Chen; Li, Shi-Hui; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 689–691; doi:10.1515/ncrs-2021-0041

data_8104802
_publ_section_title
;
 Crystal structure of catena-poly[tetraaqua-(\m2-4,4&#x2032;-bipyridine-k2
 N:N&#x2032;)-bis(\m2-4&#x2032;-methyl-[1,1&#x2032;-biphenyl]-3,5-dicarboxylato-k4
 O,O&#x2032;:O&#x2033;,O&#x2032;&#x2033;)dicadmium(II)] dihydrate,
 C20H20NO7Cd
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              689
_journal_page_last               691
_journal_paper_doi               10.1515/ncrs-2021-0041
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C20 H18 Cd N O6, H2 O'
_chemical_formula_sum            'C20 H18 Cd N O7'
_chemical_formula_weight         496.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                110.528(9)
_cell_angle_beta                 93.830(7)
_cell_angle_gamma                107.307(8)
_cell_formula_units_Z            2
_cell_length_a                   9.9506(8)
_cell_length_b                   10.1867(11)
_cell_length_c                   11.2774(11)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0940
_cell_measurement_theta_min      3.5060
_cell_volume                     1003.17(19)
_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  '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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -81.00   3.00   1.00    1.10    --  -13.48 -57.00  60.00   84
  2  \w    -83.00   5.00   1.00    1.10    --  -13.48 -38.00  90.00   88
  3  \w    -20.00  25.00   1.00    1.10    --  -13.48 -99.00 -30.00   45
  4  \w    -83.00   5.00   1.00    1.10    --  -13.48 -38.00-180.00   88
  5  \w    -32.00  56.00   1.00    1.10    --  -13.48  38.00-150.00   88
  6  \w     35.00  87.00   1.00    1.10    --   14.49 178.00  60.00   52
  7  \w     34.00  87.00   1.00    1.10    --   14.49-178.00  30.00   53
;
_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      -0.0682180000
_diffrn_orient_matrix_UB_12      -0.0329596000
_diffrn_orient_matrix_UB_13      -0.0413250000
_diffrn_orient_matrix_UB_21      -0.0331086000
_diffrn_orient_matrix_UB_22      0.0181569000
_diffrn_orient_matrix_UB_23      0.0544244000
_diffrn_orient_matrix_UB_31      0.0060425000
_diffrn_orient_matrix_UB_32      0.0696511000
_diffrn_orient_matrix_UB_33      -0.0034919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9906
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55380
_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            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.384
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3720
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+4.2966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                2947
_reflns_number_total             3720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_j_ncrs-2021-0041_suppl.cif
_cod_data_source_block           6
_cod_original_cell_volume        1003.18(17)
_cod_database_code               8104802
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C19 \\sim C7 \\sim C6 \\sim C12 \\sim C10 \\sim C11 \\sim C13
\\sim C3 \\sim C5 \\sim C16 \\sim C4 \\sim C20 \\sim C1 \\sim C15 \\sim C14
\\sim C2 \\sim C18 \\sim C17: within 7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Riding coordinates:
 O2(H2A,H2B), O1(H1A,H1B)
3.b Rotating group:
 O3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C10(H10), C5(H5), C4(H4), C1(H1), C15(H15), C14(H14),
 C2(H2), C18(H18), C17(H17)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;