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_1565547
_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         'C9.01 H12.02 Cl3 Cr N6.01'
_chemical_formula_sum            'C9.01 H12.02 Cl3 Cr N6.01'
_chemical_formula_weight         362.81
_chemical_name_systematic        mer-Cr(pzH)3Cl3
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.3070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0315(6)
_cell_length_b                   14.2944(9)
_cell_length_c                   11.3175(10)
_cell_measurement_reflns_used    8189
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      3.07
_cell_volume                     1449.22(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      297.03
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9746
_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         28.331
_diffrn_reflns_theta_min         2.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1030 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.8980. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0342P)^2^+1.2304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1596
_reflns_number_total             1805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           jlp003_b
_cod_database_code               1565547
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 1*[Sof(N4)+Sof(H4)+Sof(C4)+Sof(H4A)]+1*[Sof(N4)+Sof(H4)+Sof(C4)+Sof(H4A)]=1
 with esd of 0.01
 Sof(N4)=Sof(H4)=Sof(C4)=Sof(H4A)=FVAR(1)
 Sof(C5B)=Sof(H5B)=1-FVAR(2)
 Sof(C5A)=Sof(H5A)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2A), C3(H3), C4(H4A), C5B(H5B)
;
_shelx_res_checksum              60184
_shelx_hkl_checksum              72325
_olex2_submission_special_instructions 'No special instructions were received'