Doubly mononuclear cocrystal and oxalato-bridged binuclear copper compounds containing flexible 2-((3,5,6-trichloropyridin-2-yl)oxy)acetate tectons: Synthesis, crystal analysis and magnetic properties
Li, Jun-Xia; Du, Zhong-Xiang; Zhang, Lu-Lu; Liu, Duo-Li; Pan, Qiu-Yue; Inorganica Chimica Acta 512 (2020) 119890–; doi:10.1016/j.ica.2020.119890

data_1564114
_publ_section_title
;
 Doubly mononuclear cocrystal and oxalato-bridged binuclear copper
 compounds containing flexible 2-((3,5,6-trichloropyridin-2-yl)oxy)acetate
 tectons: Synthesis, crystal analysis and magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119890
_journal_paper_doi               10.1016/j.ica.2020.119890
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety         'C14 H14 Cl6 Cu N2 O10, C14 H10 Cl6 Cu N2 O8'
_chemical_formula_sum            'C28 H24 Cl12 Cu2 N4 O18'
_chemical_formula_weight         1256.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 98.136(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2945(5)
_cell_length_b                   6.0859(2)
_cell_length_c                   37.7878(9)
_cell_measurement_reflns_used    7664
_cell_measurement_temperature    290.2(3)
_cell_measurement_theta_max      27.3940
_cell_measurement_theta_min      3.7170
_cell_volume                     4392.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_temperature      290.2(3)
_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 0.832
_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    -72.00 -38.00   1.00   15.00    --  -13.49-178.00  90.00   34
  2  \w    -49.00  23.00   1.00   15.00    --   14.89 -57.00  60.00   72
  3  \w     35.00  73.00   1.00   15.00    --   14.89 178.00   0.00   38
  4  \w      1.00  84.00   1.00   15.00    --   14.89  38.00  30.00   83
;
_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      -0.0314131000
_diffrn_orient_matrix_UB_12      0.0150415000
_diffrn_orient_matrix_UB_13      -0.0119840000
_diffrn_orient_matrix_UB_21      -0.0147729000
_diffrn_orient_matrix_UB_22      0.0574931000
_diffrn_orient_matrix_UB_23      0.0134409000
_diffrn_orient_matrix_UB_31      0.0132005000
_diffrn_orient_matrix_UB_32      0.1003134000
_diffrn_orient_matrix_UB_33      -0.0059122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            10197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.458
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_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     294
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0288P)^2^+2.0683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3781
_reflns_number_total             4619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119890.cif
_cod_data_source_block           cu
_cod_database_code               1564114
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.696
_reflns_odcompleteness_completeness 99.68
_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
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B), O5(H5A,H5B), O9(H9A,H9B)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11)
;
_shelx_res_checksum              96001
_shelx_hkl_checksum              83579