Ligand control of low-frequency electron paramagnetic resonance linewidth in Cr(III) complexes.
Campanella, Anthony J.; Nguyen, Manh-Thuong; Zhang, Jun; Ngendahimana, Thacien; Antholine, William E.; Eaton, Gareth R.; Eaton, Sandra S.; Glezakou, Vassiliki-Alexandra; Zadrozny, Joseph M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5342–5350; doi:10.1039/d1dt00066g

data_7706980
_publ_section_title
;
 Ligand control of low-frequency electron paramagnetic resonance linewidth
 in Cr(III) complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5342
_journal_page_last               5350
_journal_paper_doi               10.1039/d1dt00066g
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H42 Cr N6, 3(Cl), 5(H2 O)'
_chemical_formula_sum            'C18 H52 Cl3 Cr N6 O5'
_chemical_formula_weight         591.01
_chemical_name_systematic
Tris((1S,2S)-(+)-1,2-diaminocyclohexane)Chromium(III)ChloridePentahydrate
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-21 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.2492(5)
_cell_length_b                   12.2492(5)
_cell_length_c                   33.5991(16)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.132
_cell_measurement_theta_min      2.647
_cell_volume                     4365.9(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            19578
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         1.920
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0751 before and 0.0677 after correction. The Ratio of minimum to maximum transmission is 0.8784. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             1902.0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.836
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 1965 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0768P)^2^+8.5074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4636
_reflns_number_total             5157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00066g2.cif
_cod_data_source_block           jz61_0m_022520_2_a
_cod_depositor_comments
'Adding full bibliography for 7706979--7706982.cif.'
_cod_original_cell_volume        4365.9(4)
_cod_database_code               7706980
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O00M-HE
 2.148 with sigma of 0.01
 Cl02-H12
 2.377 with sigma of 0.01
3.a Free rotating group:
 O00E(H8,H), O00F(H9,HA), O00J(H10,HB), O00M(H11,HC), O00Q(H12,HE)
3.b Ternary CH refined with riding coordinates:
 C00B(H00M), C00C(H00N), C00D(H00O), C00G(H00P), C00O(H00Z), C00P(H00)
3.c Secondary CH2 refined with riding coordinates:
 N005(H00A,H00B), N006(H00C,H00D), N007(H00E,H00F), N008(H00G,H00H), N009(H00I,
 H00J), N00A(H00K,H00L), C00H(H00Q,H00R), C00I(H00S,H00T), C00K(H00U,H00V),
 C00L(H00W,H00X), C00N(H00Y,HD), C00R(H1,HF), C00S(H2,HG), C00T(H3,HH), C00U(H4,
 HI), C00V(H5,HJ), C00W(H6,HK), C00X(H7,HL)
;
_shelx_res_checksum              82011
_olex2_submission_special_instructions 'No special instructions were received'