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_1564115
_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         'C36 H22 Cl6 Cu2 N6 O10, 2(C2 H6 O)'
_chemical_formula_sum            'C40 H34 Cl6 Cu2 N6 O12'
_chemical_formula_weight         1130.51
_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     iterative
_cell_angle_alpha                94.019(4)
_cell_angle_beta                 102.129(5)
_cell_angle_gamma                106.347(5)
_cell_formula_units_Z            1
_cell_length_a                   7.7129(4)
_cell_length_b                   9.8035(5)
_cell_length_c                   16.0541(9)
_cell_measurement_reflns_used    2884
_cell_measurement_temperature    291.2(2)
_cell_measurement_theta_max      25.2530
_cell_measurement_theta_min      3.9230
_cell_volume                     1127.97(11)
_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_temperature      291.2(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 0.826
_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    -12.00  14.00   1.00   10.00    --  -13.80  19.00-180.00   26
  2  \w    -30.00   8.00   1.00   10.00    --  -13.80 -86.00 114.00   38
  3  \w    -28.00  52.00   1.00   10.00    --  -13.80  57.00  90.00   80
  4  \w    -12.00  19.00   1.00   10.00    --  -13.80 -99.00   0.00   31
  5  \w    -52.00  42.00   1.00   10.00    --   14.82 -77.00-150.00   94
  6  \w    -10.00  80.00   1.00   10.00    --   14.82  77.00 -30.00   90
;
_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      -0.0283681000
_diffrn_orient_matrix_UB_12      -0.0438393000
_diffrn_orient_matrix_UB_13      -0.0404816000
_diffrn_orient_matrix_UB_21      -0.0928127000
_diffrn_orient_matrix_UB_22      -0.0225081000
_diffrn_orient_matrix_UB_23      0.0047200000
_diffrn_orient_matrix_UB_31      -0.0181017000
_diffrn_orient_matrix_UB_32      0.0580219000
_diffrn_orient_matrix_UB_33      -0.0205102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.415
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63426
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0272P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3454
_reflns_number_total             4683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119890.cif
_cod_data_source_block           cu2
_cod_database_code               1564115
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.726
_reflns_odcompleteness_completeness 99.76
_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 C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C19(H19), C20(H20), C17(H17), C12(H12), C18(H18),
 C11(H11), C3(H3)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
2.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              79298
_shelx_hkl_checksum              2015