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_1564038
_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 Br Cu N6, Cl O4, C2 H3 N'
_chemical_formula_sum            'C32 H29 Br Cl Cu N7 O4'
_chemical_formula_weight         754.52
_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     dual
_cell_angle_alpha                74.810(3)
_cell_angle_beta                 70.818(3)
_cell_angle_gamma                72.847(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4038(11)
_cell_length_b                   11.4048(11)
_cell_length_c                   13.4610(13)
_cell_measurement_reflns_used    7743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.062
_cell_measurement_theta_min      2.368
_cell_volume                     1553.3(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'fine focused sealed tube'
_exptl_absorpt_coefficient_mu    2.126
_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    1.613
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   28.31
_exptl_transmission_factor_min   1.79
_refine_diff_density_max         1.656
_refine_diff_density_min         -2.739
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0719P)^2^+10.2991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6884
_reflns_number_total             7743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           7
_cod_database_code               1564038
_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:
 C00U(H00A,H00B), C016(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C017(H017), C019(H019)
2.c Idealised Me refined as rotating group:
 C01A(H01C,H01D,H01E)
;