Crystal structure of poly[tetraaqua-bis(μ4-5-(4-carboxy-benzylamino)-isophthalato-κ4 O,O′:O′′:O′′′)-(μ2-4,4′-di(1H-imidazol-1-yl)-1,1′-biphenyl-κ2 N:N′)dicadmium(II)], C25H22N3O8Cd
Li, Shi-Hui; Li, Guan-Feng; Zhang, Li; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1271–1273; doi:10.1515/ncrs-2020-0228

data_8105440
_publ_section_title
;
 Crystal structure of
 poly[tetraaqua-bis(\m4-5-(4-carboxy-benzylamino)-isophthalato-\k4
 O,O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)-(\m2-4,4&#x2032;-di(1H-imidazol-1-yl)-1,1&#x2032;-biphenyl-\k2
 N:N&#x2032;)dicadmium(II)], C25H22N3O8Cd
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1271
_journal_page_last               1273
_journal_paper_doi               10.1515/ncrs-2020-0228
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C25 H22 Cd N3 O8'
_chemical_formula_sum            'C25 H22 Cd N3 O8'
_chemical_formula_weight         604.86
_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     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.698(9)
_cell_angle_beta                 72.168(9)
_cell_angle_gamma                63.166(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2722(10)
_cell_length_b                   10.6897(11)
_cell_length_c                   12.5667(13)
_cell_measurement_reflns_used    3787
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7720
_cell_measurement_theta_min      3.8900
_cell_volume                     1170.8(2)
_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    -70.00  -5.00   1.00    3.50    --  -13.80 129.00 178.92   65
  2  \w    -20.00  25.00   1.00    3.50    --  -13.80 -99.00 -30.00   45
  3  \w    -84.00  16.00   1.00    3.50    --  -13.80 -19.00  30.00  100
  4  \w    -83.00   5.00   1.00    3.50    --  -13.80 -38.00 -30.00   88
  5  \w     -4.00  84.00   1.00    3.50    --   14.82  38.00 -60.00   88
  6  \w     -2.00  82.00   1.00    3.50    --   14.82  57.00 -30.00   84
  7  \w    -20.00  54.00   1.00    3.50    --   14.82 -99.00  90.00   74
  8  \w    -20.00  54.00   1.00    3.50    --   14.82 -99.00   0.00   74
  9  \w     -4.00  84.00   1.00    3.50    --   14.82  38.00-150.00   88
 10  \w    -53.00  42.00   1.00    3.50    --   14.82 -77.00-180.00   95
 11  \w    -20.00  25.00   1.00    3.50    --  -13.80 -99.00 120.00   45
;
_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      -0.0794452000
_diffrn_orient_matrix_UB_12      0.0392305000
_diffrn_orient_matrix_UB_13      0.0116103000
_diffrn_orient_matrix_UB_21      0.0091121000
_diffrn_orient_matrix_UB_22      0.0450146000
_diffrn_orient_matrix_UB_23      -0.0477250000
_diffrn_orient_matrix_UB_31      -0.0040917000
_diffrn_orient_matrix_UB_32      -0.0444667000
_diffrn_orient_matrix_UB_33      -0.0333261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19983
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63606
_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_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                3318
_reflns_number_total             4352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0228_suppl.cif
_cod_data_source_block           s2
_cod_database_code               8105440
_chemical_oxdiff_formula         'C H N  O CD'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Rotating group:
 O1(H1A), O2(H2A)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12),
 C14(H14), C16(H16), C20(H20), C21(H21), C23(H23), C24(H24)
2.d Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_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 2.688
_oxdiff_exptl_absorpt_empirical_full_min 0.478