Five-coordinate [(L2)2CuII(X)]z+ (X = H2O, z = 2; X = N3−, SCN−, NO2−, MeCO2−, Cl−, Br−, z = 1; L2 = 1-benzyl-[3-(2-pyridyl)]pyrazole) complexes: Structural index, EPR and redox potential correlations
Mukherjee, Jhumpa; Sengupta, Arunava; Mukherjee, Rabindranath; Inorganica Chimica Acta 513 (2020) 119899–; doi:10.1016/j.ica.2020.119899

data_1564037
_publ_section_title
;
 Five-coordinate [(L2)2CuII(X)]z+ (X&#x00A0;=&#x00A0;H2O,
 z&#x00A0;=&#x00A0;2; X&#x00A0;=&#x00A0;N3&#x2212;, SCN&#x2212;,
 NO2&#x2212;, MeCO2&#x2212;, Cl&#x2212;, Br&#x2212;, z&#x00A0;=&#x00A0;1;
 L2&#x00A0;=&#x00A0;1-benzyl-[3-(2-pyridyl)]pyrazole) complexes:
 Structural index, EPR and redox potential correlations
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119899
_journal_paper_doi               10.1016/j.ica.2020.119899
_journal_volume                  513
_journal_year                    2020
_chemical_formula_moiety         'C30 H26 Cl Cu N6, Cl O4, C2 H3 N'
_chemical_formula_sum            'C32 H29 Cl2 Cu N7 O4'
_chemical_formula_weight         710.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 106.626(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9709(13)
_cell_length_b                   15.0437(15)
_cell_length_c                   15.3931(14)
_cell_measurement_reflns_used    7697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.062
_cell_measurement_theta_min      2.368
_cell_volume                     3100.0(5)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_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_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         2.694
_diffrn_source                   'fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.694942
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   28.31
_exptl_transmission_factor_min   1.79
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0136P)^2^+5.1108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6035
_reflns_number_total             7697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           6
_cod_database_code               1564037
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.912
_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
2.a Secondary CH2 refined with riding coordinates:
 C00T(H00A,H00B), C011(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012), C014(H014),
 C016(H016), C017(H017), C018(H018), C01A(H01C)
2.c Idealised Me refined as rotating group:
 C019(H01D,H01E,H01F)
;