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_1564032
_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 H28 Cu N6 O, 2(Cl O4)'
_chemical_formula_sum            'C30 H28 Cl2 Cu N6 O9'
_chemical_formula_weight         751.02
_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                 93.303(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.986(5)
_cell_length_b                   13.871(5)
_cell_length_c                   20.060(5)
_cell_measurement_reflns_used    5905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.062
_cell_measurement_theta_min      2.368
_cell_volume                     3051.8(19)
_computing_cell_refinement       'SAINT V6.36A (?, 2016)'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'SAINT V6.36A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.694942
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.0444 before and 0.0278 after correction.
The Ratio of minimum to maximum transmission is 0.6949.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   28.31
_exptl_transmission_factor_min   1.79
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0450P)^2^+4.6913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4790
_reflns_number_total             5381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1-L2H2O
_cod_database_code               1564032
_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
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C26(H26), C1(H1), C11(H11), C7(H7), C4(H4), C15(H15), C19(H19),
 C8(H8), C30(H30), C17(H17), C28(H28), C3(H3), C22(H22), C12(H12), C23(H23),
 C14(H14), C27(H27), C2(H2), C16(H16), C13(H13), C18(H18)
;