The crystal structure of catena-poly[aqua-(4-iodopyridine-2,6-dicarboxylato-κ 3 N,O,O ′)-copper(II)] monohydrate, C7H6NO6ICu
Kong, Yang; Lu, ChenFei; Wang, Chang-Zhao; Tian, Bin; Dang, YiXuan; Han, ZiHao; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1057–1059; doi:10.1515/ncrs-2023-0296

data_8107659
_publ_section_title
;
 The crystal structure of
 catena-poly[aqua-(4-iodopyridine-2,6-dicarboxylato-\k 3 N,O,O
 &#x2032;)-copper(II)] monohydrate, C7H6NO6ICu
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1057
_journal_page_last               1059
_journal_paper_doi               10.1515/ncrs-2023-0296
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C7 H4 Cu I N O5, H2 O'
_chemical_formula_sum            'C7 H6 Cu I N O6'
_chemical_formula_weight         390.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.636(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7229(4)
_cell_length_b                   5.1728(2)
_cell_length_c                   20.8336(8)
_cell_measurement_reflns_used    4895
_cell_measurement_temperature    292.7(3)
_cell_measurement_theta_max      25.9940
_cell_measurement_theta_min      4.2160
_cell_volume                     1038.53(7)
_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      292.7(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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    -79.00  60.00   1.00    5.00    --   -9.62   0.00  30.00  139
  2  \w    -77.00  17.00   1.00    5.00    --   -9.62 -77.00  30.00   94
  3  \w    -26.00   1.00   1.00    5.00    --   -9.62  57.00 150.00   27
  4  \w    -20.00   5.00   1.00    5.00    --   -9.62 -99.00  30.00   25
  5  \w     -6.00  20.00   1.00    5.00    --   -9.62 -99.00-150.00   26
  6  \w      8.00  34.00   1.00    5.00    --   10.64  57.00-180.00   26
  7  \w    -22.00  27.00   1.00    5.00    --   10.64 -94.00-133.00   49
  8  \w    -26.00  50.00   1.00    5.00    --   -9.62  57.00  60.00   76
;
_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      -0.0689864000
_diffrn_orient_matrix_UB_12      -0.0216492000
_diffrn_orient_matrix_UB_13      0.0062812000
_diffrn_orient_matrix_UB_21      -0.0255063000
_diffrn_orient_matrix_UB_22      0.0466114000
_diffrn_orient_matrix_UB_23      -0.0313565000
_diffrn_orient_matrix_UB_31      0.0024154000
_diffrn_orient_matrix_UB_32      -0.1270862000
_diffrn_orient_matrix_UB_33      -0.0125812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9029
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.401
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.088
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43378
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.498
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.421
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0328P)^2^+1.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1642
_reflns_number_total             1790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0296_suppl_001.cif
_cod_data_source_block           521b7
_cod_original_cell_volume        1038.52(7)
_cod_database_code               8107659
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_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.a Free rotating group:
 O6(H6A,H6B)
2.b Rotating group:
 O5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
;
_shelx_res_checksum              90461
_shelx_hkl_checksum              36136
_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 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.559