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_1565550
_publ_section_title
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 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         'C9 H9 Cl6 Cr N6'
_chemical_formula_sum            'C9 H9 Cl6 Cr N6'
_chemical_formula_weight         465.92
_chemical_name_systematic        mer-CrCl3(4-Cl-pzH)3
_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   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                78.808(15)
_cell_angle_beta                 89.621(15)
_cell_angle_gamma                88.186(15)
_cell_formula_units_Z            2
_cell_length_a                   6.792(3)
_cell_length_b                   10.395(3)
_cell_length_c                   12.218(4)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      2.87
_cell_volume                     845.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      295.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16370
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.304
_diffrn_reflns_theta_min         2.864
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  0.9014
_exptl_absorpt_correction_T_min  0.7824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0435 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.8680. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear grayish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       cubic
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0292P)^2^+0.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2900
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           jlp068_a
_cod_original_cell_volume        845.7(5)
_cod_database_code               1565550
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl5B(0.45) Cl5A(0.55)
;
_shelx_res_checksum              4083
_shelx_hkl_checksum              58268
_olex2_submission_special_instructions 'No special instructions were received'