Chromium(III)-pyrazole complexes. X-Ray crystal structures, 1H NMR investigation of ligand fluxional behavior and EPR studies
López Plá, Jessica M.; Boudalis, Athanassios K.; Telser, Joshua; Raptis, Raphael G.; Inorganica Chimica Acta 502 (2020) 119299–; doi:10.1016/j.ica.2019.119299

data_1565553
_publ_section_title
;
 Chromium(III)-pyrazole complexes. X-Ray crystal structures, 1H NMR
 investigation of ligand fluxional behavior and EPR studies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119299
_journal_paper_doi               10.1016/j.ica.2019.119299
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         '2(C6 H8 Cl Cr0.5 N4), Cl'
_chemical_formula_sum            'C12 H16 Cl3 Cr N8'
_chemical_formula_weight         430.68
_chemical_name_systematic        '[trans-Cr(pzH)4Cl2]Cl'
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                76.6970(10)
_cell_angle_beta                 89.9270(10)
_cell_angle_gamma                68.3690(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0428(3)
_cell_length_b                   8.4370(4)
_cell_length_c                   14.9426(6)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.96
_cell_volume                     913.34(7)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 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      302.21
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19464
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         2.959
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0672 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.9209. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       needle
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.6702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2961
_reflns_number_total             3729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           jlp035_0m_a
_cod_database_code               1565553
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.863
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1), N3(H3), N5(H5A), N7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7A), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              38391
_shelx_hkl_checksum              43358
_olex2_submission_special_instructions 'No special instructions were received'