Crystal structure of [aqua-(4-iodopyridine-2,6-dicarboxylato-κ3 O,N,O′)-(1,10-phenanothroline-κ2 N,N′)copper(II)] dihydrate, C19H16O7N3CuI
Lv, Benlian; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 891–893; doi:10.1515/ncrs-2021-0119

data_8104616
_publ_section_title
;
 Crystal structure of [aqua-(4-iodopyridine-2,6-dicarboxylato-\k3
 O,N,O&#x2032;)-(1,10-phenanothroline-\k2 N,N&#x2032;)copper(II)]
 dihydrate, C19H16O7N3CuI
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              891
_journal_page_last               893
_journal_paper_doi               10.1515/ncrs-2021-0119
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C19 H12 Cu I N3 O5, 2(H2 O)'
_chemical_formula_sum            'C19 H16 Cu I N3 O7'
_chemical_formula_weight         588.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5772(2)
_cell_length_b                   17.3473(3)
_cell_length_c                   18.8445(3)
_cell_measurement_reflns_used    29604
_cell_measurement_temperature    289.32(10)
_cell_measurement_theta_max      26.3950
_cell_measurement_theta_min      3.8080
_cell_volume                     4111.50(12)
_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      289.32(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 0.997
_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    -77.00   7.00   1.00    4.00    --   -9.62 -57.00  60.00   84
  2  \w    -81.00  20.00   1.00    4.00    --   -9.62 -19.00-180.00  101
  3  \w     -6.00  78.00   1.00    4.00    --   10.64  57.00   0.00   84
  4  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00 -60.00   70
  5  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00  30.00   70
  6  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00 150.00   70
  7  \w     -6.00  78.00   1.00    4.00    --   10.64  57.00-150.00   84
  8  \w    -57.00  37.00   1.00    4.00    --   10.64 -77.00-150.00   94
  9  \w    -20.00  29.00   1.00    4.00    --   -9.62 -99.00-180.00   49
 10  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00 -30.00   70
 11  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00 120.00   70
 12  \w    -20.00  50.00   1.00    4.00    --   10.64 -99.00-120.00   70
;
_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      -0.0283940000
_diffrn_orient_matrix_UB_12      -0.0213565000
_diffrn_orient_matrix_UB_13      -0.0259169000
_diffrn_orient_matrix_UB_21      -0.0105300000
_diffrn_orient_matrix_UB_22      -0.0291286000
_diffrn_orient_matrix_UB_23      0.0254523000
_diffrn_orient_matrix_UB_31      -0.0475737000
_diffrn_orient_matrix_UB_32      0.0191829000
_diffrn_orient_matrix_UB_33      0.0098319000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71115
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.446
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68937
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0345P)^2^+7.3813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3385
_reflns_number_total             3611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0119_suppl.cif
_cod_data_source_block           lls-1020-2
_cod_database_code               8104616
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.508
_reflns_odcompleteness_completeness 99.46
_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), O7(H7A,H7B)
2.b Rotating group:
 O5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C8(H8), C14(H14), C9(H9), C10(H10), C15(H15), C19(H19),
 C16(H16), C18(H18)
;