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_7706979
_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((1R,2R)-(+)-1,2-diaminocyclohexane)Chromium(III)ChloridePentahydrate
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-17
_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                   12.2603(6)
_cell_length_b                   12.2603(6)
_cell_length_c                   33.2599(16)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.28
_cell_volume                     4329.7(4)
_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      100.0
_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  0.0669
_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       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            171415
_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         26.365
_diffrn_reflns_theta_min         2.013
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0778 before and 0.0719 after correction. The Ratio of minimum to maximum transmission is 0.8536. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             1902.0
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2577 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5915
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0347P)^2^+12.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5588
_reflns_number_total             5914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00066g2.cif
_cod_data_source_block           jz66_0m03092020_a
_cod_depositor_comments
'Adding full bibliography for 7706979--7706982.cif.'
_cod_original_cell_volume        4329.7(5)
_cod_database_code               7706979
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, 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
 Cl03-HG
 2.482 with sigma of 0.02
 Cl-H6
 2.234 with sigma of 0.02
 O0AA-H00B
 2.174 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C00E, C00V, C0AA, C00Z, C1AA, C00F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00S, C00G, C00H, C00D, C00Q, C00I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00N, C00K, C00X, C00O, C00M, C00C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O1A)=Sof(H1AE)=Sof(H1AF)=Sof(O1AB)=Sof(H1AG)=Sof(H1AH)=1-FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=Sof(O1AA)=Sof(H1AC)=Sof(H1AD)=FVAR(1)
 Sof(Cl1A)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
5.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AC,H0AD), O1AA(H1AC,H1AD), O1A(H1AE,H1AF), O1AB(H1AG,
 H1AH), O00L(H6,HF), O00U(H7,HG)
5.b Ternary CH refined with riding coordinates:
 C00C(H00M), C00D(H00N), C00E(H00O), C00F(H00P), C00H(H00S), C00N(H00Z)
5.c Secondary CH2 refined with riding coordinates:
 N005(H00A,H00B), N006(H00C,H00D), N007(H00E,H00F), N008(H00G,H00H), N00A(H00I,
 H00J), N00B(H00K,H00L), C00G(H00Q,H00R), C00I(H00T,H00U), C00K(H00V,H00W),
 C00M(H00X,H00Y), C00O(H00,H), C00Q(H1,HA), C00S(H2,HB), C00X(H3,HC), C0AA(H0AA,
 H0AB), C00Z(H4,HD), C1AA(H1AA,H1AB), C00V(H5,HE)
;
_shelx_res_checksum              8383
_olex2_submission_special_instructions 'No special instructions were received'