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_1565549
_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         'C12 H18 Cl3 Cr N6'
_chemical_formula_sum            'C12 H18 Cl3 Cr N6'
_chemical_formula_weight         404.67
_chemical_name_systematic        mer-CrCl3(4-Me-pzH)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.356(2)
_cell_length_b                   11.590(2)
_cell_length_c                   13.632(3)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.92
_cell_volume                     1794.2(6)
_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      273.15
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Quest Bruker'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.451
_diffrn_reflns_theta_min         2.922
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0732 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.9238. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0398P)^2^+0.7674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.752
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2922
_reflns_number_total             3684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           aa_a_pl
_cod_database_code               1565549
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.051) H4(0.05) H6(0.048) H1(0.051) H3(0.059) H4A(0.124)
 H4B(0.124) H4C(0.124) H5(0.053) H7(0.056) H8A(0.102) H8B(0.102) H8C(0.102)
 H9(0.041) H11(0.064) H12A(0.101) H12B(0.101) H12C(0.101)
 Fixed X: H2(-0.483814) H4(-0.238516) H6(-0.503305) H1(-0.566927) H3(-
 0.640853) H4A(-0.717236) H4B(-0.809018) H4C(-0.73755) H5(-0.155433) H7(-
 0.090219) H8A(0.076351) H8B(-0.02158) H8C(0.018834) H9(-0.286124) H11(-
 0.502921) H12A(-0.401606) H12B(-0.349958) H12C(-0.269168)
 Fixed Y: H2(0.701019) H4(0.433837) H6(0.233595) H1(0.439687) H3(0.764802)
 H4A(0.65479) H4B(0.616059) H4C(0.523216) H5(0.263169) H7(0.302794)
 H8A(0.18783) H8B(0.09454) H8C(0.125441) H9(0.323126) H11(0.078182)
 H12A(0.116996) H12B(0.02164) H12C(0.12224)
 Fixed Z: H2(-0.359563) H4(-0.149879) H6(-0.342507) H1(-0.512745) H3(-
 0.460144) H4A(-0.642404) H4B(-0.563065) H4C(-0.621797) H5(-0.366213) H7(-
 0.085917) H8A(-0.257629) H8B(-0.27432) H8C(-0.167543) H9(-0.547616) H11(-
 0.458843) H12A(-0.677142) H12B(-0.607852) H12C(-0.644998)
;
_shelx_res_checksum              45022
_shelx_hkl_checksum              4548
_olex2_submission_special_instructions 'No special instructions were received'