Crystal structure of catena-poly[bis(µ2-3,5-bis(1-imidazolyl)pyridine-κ2 N:N′)-(µ2-3-nitrophthalato-k3 O,O′:O″)cadmium(II)] dihydrate, C30H25N11O8Cd
Yin, Wei-Dong; Liu, Qian-Long; Zhao, Ya-Jing; Gong, Xiao-Ru; Li, Gui-Lian; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 899–902; doi:10.1515/ncrs-2021-0133

data_8104618
_publ_section_title
;
 Crystal structure of
 catena-poly[bis(&#x00B5;2-3,5-bis(1-imidazolyl)pyridine-\k2
 N:N&#x2032;)-(&#x00B5;2-3-nitrophthalato-k3
 O,O&#x2032;:O&#x2033;)cadmium(II)] dihydrate, C30H25N11O8Cd
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              899
_journal_page_last               902
_journal_paper_doi               10.1515/ncrs-2021-0133
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C30 H21 Cd1 N11 O6, 2H2 O'
_chemical_formula_sum            'C30 H25 Cd N11 O8'
_chemical_formula_weight         780.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9344(3)
_cell_length_b                   18.2722(3)
_cell_length_c                   9.5619(2)
_cell_measurement_reflns_used    15830
_cell_measurement_temperature    293.28(10)
_cell_measurement_theta_max      27.2020
_cell_measurement_theta_min      3.8270
_cell_volume                     3133.44(10)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.28(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.928
_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  25.00   1.00    3.39    --  -13.80 -99.00 -90.00   45
  2  \w    -83.00   5.00   1.00    3.39    --  -13.80 -38.00   0.00   88
  3  \w    -86.00 -35.00   1.00    3.39    --  -13.80-178.00-120.00   51
  4  \w    -20.00  25.00   1.00    3.39    --  -13.80 -99.00 150.00   45
  5  \w     -4.00  84.00   1.00    3.39    --   14.82  38.00-120.00   88
  6  \w     -2.00  82.00   1.00    3.39    --   14.82  57.00 -60.00   84
  7  \w    -17.00  47.00   1.00    3.39    --   14.82 -99.00  60.00   64
  8  \w     -4.00  84.00   1.00    3.39    --   14.82  38.00-180.00   88
;
_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      -0.0346833000
_diffrn_orient_matrix_UB_12      0.0239042000
_diffrn_orient_matrix_UB_13      0.0138719000
_diffrn_orient_matrix_UB_21      0.0120925000
_diffrn_orient_matrix_UB_22      0.0701962000
_diffrn_orient_matrix_UB_23      -0.0041103000
_diffrn_orient_matrix_UB_31      -0.0147375000
_diffrn_orient_matrix_UB_32      0.0012127000
_diffrn_orient_matrix_UB_33      -0.0360013000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35240
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.448
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84166
_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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3786
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0217P)^2^+2.8369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3390
_reflns_number_total             3786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0133_suppl.cif
_cod_data_source_block           lgl-44
_cod_original_formula_sum        'C30 H25 Cd1 N11 O8'
_cod_database_code               8104618
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.754
_reflns_odcompleteness_completeness 99.57
_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,H) groups
2. Restrained distances
 N6-O4 \\sim N6-O4A
 with sigma of 0.01
 N6-O5 \\sim N6-O5A
 with sigma of 0.01
3. Rigid bond restraints
 O4, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O5A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O4A)=Sof(O5A)=0.5*(1-FVAR(2))
 Sof(O4)=Sof(O5)=0.5*FVAR(2)
6.a Riding coordinates:
 O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19)
;
_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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.791