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_7706982
_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
'2(C42 H48 Cr N6), 6(Cl), 2(C2 H6 O S), 5(C H4 O), C2 H6 O'
_chemical_formula_sum            'C96 H138 Cl6 Cr2 N12 O9 S2'
_chemical_formula_weight         1985.00
_chemical_name_systematic
Tris((1R,2R)-(-)-1,2-diphenylethylenediamine)Chromium(III)Chloride
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                 104.287(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3901(5)
_cell_length_b                   19.3151(8)
_cell_length_c                   24.4122(11)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      0.86
_cell_volume                     5661.5(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      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            151263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.710
_diffrn_reflns_theta_max         24.710
_diffrn_reflns_theta_min         0.861
_exptl_absorpt_coefficient_mu    0.424
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             2104.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Flack x determined using 7276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1158
_refine_ls_number_reflns         19285
_refine_ls_number_restraints     762
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0853
_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^)+(0.1837P)^2^+10.5122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2412
_refine_ls_wR_factor_ref         0.2622
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                16763
_reflns_number_total             19288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00066g2.cif
_cod_data_source_block           jz90_0m100520_a
_cod_depositor_comments
'Adding full bibliography for 7706979--7706982.cif.'
_cod_database_code               7706982
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.884
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C4A-O3
 1.45 with sigma of 0.02
 C2-O2
 1.45 with sigma of 0.02
 C23-O0
 1.45 with sigma of 0.02
 O00B-C033
 1.43 with sigma of 0.02
 O2-C2
 1.43 with sigma of 0.01
 O0-C23
 1.43 with sigma of 0.01
 O01U-C5
 1.43 with sigma of 0.01
 O3-C4A
 1.43 with sigma of 0.01
 O02U-C03N
 1.43 with sigma of 0.01
 S1A-C1A
 1.4 with sigma of 0.005
 S1A-C1A = S1A-C4
 1.78 with sigma of 0.02
 C021-C02E \\sim C01J-C028 \\sim C034-C027
 with sigma of 0.02
 C02C-C3 \\sim C01P-C02J \\sim C6-C7
 with sigma of 0.02
 C00X-C02Q \\sim C01G-C018 \\sim C02W-C01M
 with sigma of 0.02
 C010-C02F \\sim C02G-C01E \\sim C026-C01X
 with sigma of 0.02
 C00J-C00R \\sim C016-C015 \\sim C024-C01Y
 with sigma of 0.02
 C011-C00Z \\sim C01O-C02Z \\sim C02H-C025
 with sigma of 0.02
 C011-C025 \\sim C02H-C02Z \\sim C01O-C00Z
 with sigma of 0.02
 C01Y-C024 \\sim C015-C016 \\sim C00R-C00J
 with sigma of 0.02
 C00M-C01U \\sim C01K-C02V \\sim C02D-C02X
 with sigma of 0.02
 C02T-C01S \\sim C02P-C02O \\sim C02M-C022
 with sigma of 0.02
 C00U-C029 \\sim C023-C02S \\sim C035-C02B
 with sigma of 0.02
 C00O-C00W \\sim C01L-C014 \\sim C01A-C00Q
 with sigma of 0.02
 C0-C1AA \\sim C03G-C03F \\sim C038-C0AA
 with sigma of 0.02
 O00D-C032 \\sim S1A-C1A
 with sigma of 0.02
 O02U-C03N \\sim O013-C03A \\sim O0-C23
 with sigma of 0.02
 O00B-C033 \\sim O02U-C03N \\sim O00D-C032 \\sim O3-C4A \\sim O01U-C5 \\sim
O012-C030 \\sim O0-C23 ~
 O013-C03A \\sim S1A-C1A \\sim O2-C2
 with sigma of 0.02
 C026-C01X \\sim C026-C01E \\sim C02G-C01E \\sim C02G-C02F \\sim C02F-C010
\\sim C01X-C010 \\sim C02Q-
 C00X \\sim C02Q-C01G \\sim C01G-C018 \\sim C02W-C018 \\sim C02W-C01M \\sim
C01M-C00X
 with sigma of 0.02
 C025-C011 \\sim C02H-C025 \\sim C02Z-C02H \\sim C02Z-C01O \\sim C01O-C00Z
\\sim C011-C00Z \\sim C01Y-
 C00J \\sim C024-C01Y \\sim C024-C015 \\sim C016-C015 \\sim C016-C00R \\sim
C00R-C00J \\sim C3-C02C ~
 C3-C01P \\sim C02J-C01P \\sim C6-C02J \\sim C7-C6 \\sim C7-C02C \\sim
C027-C021 \\sim C034-C027 \\sim C034-
 C028 \\sim C028-C01J \\sim C02E-C01J \\sim C02E-C021
 with sigma of 0.02
 C02X-C00M \\sim C02X-C02D \\sim C02V-C01K \\sim C01U-C01K \\sim C01U-C00M
\\sim C02V-C02D \\sim C02P-
 C01S \\sim C02P-C02O \\sim C02O-C02M \\sim C02M-C022 \\sim C02T-C022 \\sim
C02T-C01S
 with sigma of 0.02
 C01W-C00Y \\sim C01W-C01C \\sim C01C-C017 \\sim C01R-C017 \\sim C01R-C01N
\\sim C01N-C00Y \\sim C0AA-
 C038 \\sim C0AA-C0 \\sim C1AA-C0 \\sim C1AA-C03G \\sim C03G-C03F \\sim
C03F-C038
 with sigma of 0.02
 C035-C02S \\sim C035-C02B \\sim C02S-C023 \\sim C029-C023 \\sim C029-C00U
\\sim C02B-C00U
 with sigma of 0.02
 O0-C23 \\sim O013-C03A
 with sigma of 0.02
 C00R-C00J \\sim C016-C00R \\sim C016-C015 \\sim C024-C015 \\sim C024-C01Y
\\sim C01Y-C00J
 with sigma of 0.015
 C029-C023 \\sim C029-C00U \\sim C035-C02S \\sim C02B-C00U \\sim C035-C02B
\\sim C02S-C023
 with sigma of 0.015
 C03G-C03F \\sim C1AA-C03G \\sim C1AA-C0 \\sim C0AA-C0 \\sim C03F-C038 \\sim
C0AA-C038
 with sigma of 0.01
 C02P-C01S \\sim C02P-C02O \\sim C02O-C02M \\sim C02M-C022 \\sim C02T-C022
\\sim C02T-C01S
 with sigma of 0.01
 C026-C01X \\sim C01X-C010 \\sim C02F-C010 \\sim C02G-C02F \\sim C02G-C01E
\\sim C026-C01E
 with sigma of 0.01
 C02X-C00M \\sim C02X-C02D \\sim C02V-C01K \\sim C02V-C02D \\sim C01U-C01K
\\sim C01U-C00M
 with sigma of 0.01
 C02S-C023 \\sim C029-C023 \\sim C029-C00U \\sim C02B-C00U \\sim C035-C02B
\\sim C035-C02S
 with sigma of 0.01
 C3-C01P \\sim C3-C02C \\sim C7-C6 \\sim C6-C02J \\sim C02J-C01P
 with sigma of 0.01
 S1A-C1A \\sim S1A-C4
 with sigma of 0.02
 C034-H034 \\sim C034-C027 \\sim C034-C028
 with sigma of 0.01
 S1A-O1 \\sim S07-O00L
 with sigma of 0.02
 S07-C036 \\sim S07-C03I \\sim S1A-C4 \\sim S1A-C1A
 with sigma of 0.02
3. Restrained planarity
 C01R, C01N, C00Y, C01W, C01C, C017
 with sigma of 0.1
 C0AA, C0, C1AA, C03G, C03F, C038
 with sigma of 0.1
 C00U, C029, C023, C02S, C035, C02B
 with sigma of 0.1
 C00O, C00W, C01L, C014, C01A, C00Q
 with sigma of 0.1
 C00M, C01U, C01K, C02V, C02D, C02X
 with sigma of 0.1
 C011, C00Z, C01O, C02Z, C02H, C025
 with sigma of 0.1
 C00X, C01M, C02W, C018, C01G, C02Q
 with sigma of 0.1
 C00J, C00R, C016, C015, C024, C01Y
 with sigma of 0.1
 C02C, C7, C6, C02J, C01P, C3
 with sigma of 0.1
 C01X, C010, C02F, C02G, C01E, C026
 with sigma of 0.1
 C021, C027, C034, C028, C01J, C02E
 with sigma of 0.1
 C01S, C02P, C02O, C02M, C022, C02T
 with sigma of 0.1
4. Rigid bond restraints
 C1A, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1A \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C4 \\sim C1A: within 2.5A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2.5A
C1A \\sim S1A \\sim C4: within 2.5A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2.5A
C4 \\sim S1A \\sim C1A \\sim O1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
6. Others
 Sof(H02C)=Sof(C03O)=Sof(H03D)=Sof(H03E)=Sof(H03H)=1-FVAR(1)
 Sof(H02U)=Sof(C03N)=Sof(H03A)=Sof(H03B)=Sof(H03C)=FVAR(1)
 Sof(O0)=Sof(H0A)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(2)
 Sof(O013)=Sof(H013)=Sof(C03A)=Sof(H03X)=Sof(H03Y)=Sof(H)=FVAR(2)
 Fixed Sof: O3(0.5) H3A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) O01U(0.5)
 H01R(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
7.a Ternary CH refined with riding coordinates:
 C019(H019), C01B(H01B), C01H(H01H), C01I(H01I), C01Q(H01Q), C01V(H01V),
 C01Z(H01Z), C02A(H02A), C02K(H02K), C02N(H02N), C02R(H02R), C031(H031)
7.b Secondary CH2 refined with riding coordinates:
 N00C(H00A,H00B), N00E(H00C,H00D), N00F(H00E,H00F), N00G(H00G,H00H), N00H(H00I,
 H00J), N00I(H00K,H00L), N00K(H00M,H00N), N00N(H00O,H00P), N00P(H00R,H00S),
 N00S(H00U,H00V), N00V(H00X,H00Z), N01D(H01D,H01E), C2(H2A,H2B)
7.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00R(H00T), C00W(H00W), C00Y(H00Y), C00Z(H00), C010(H010),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C01A(H01A),
 C01C(H01C), C01E(H01F), C01G(H01G), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01U(H01U), C01W(H01W),
 C01Y(H01Y), C022(H022), C023(H023), C024(H024), C025(H025), C026(H026),
 C027(H027), C028(H028), C029(H029), C02B(H02B), C02D(H02D), C02E(H02E),
 C02F(H02F), C02G(H02G), C02H(H02H), C02M(H02M), C02O(H02O), C02P(H02P),
 C02Q(H02Q), C02S(H02S), C02T(H02T), C02V(H02V), C02W(H02W), C02X(H02X),
 C02Z(H02Z), C034(H034), C035(H035), C038(H038), C03F(H03F), C0(H0), C1AA(H1AA),
  C03G(H03G), C3(H3), C02J(H02J), C6(H6), C7(H7)
7.d Tetrahedral OH refined with riding coordinates:
 O02U(H02U), O02U(H02C)
7.e Idealised Me refined as rotating group:
 C030(H03U,H03V,H03W), C032(H03R,H03S,H03T), C033(H03O,H03P,H03Q), C036(H03I,
 H03J,H03K), C03A(H03X,H03Y,H), C03I(H03L,H03M,H03N), C03N(H03A,H03B,H03C),
 C03O(H03D,H03E,H03H), C4A(H4AA,H4AB,H4AC), C1A(H1AB,H1AC,H1AD), C5(H5A,H5B,
 H5C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C4(H4A,H4B,H4C)
7.f Idealised tetrahedral OH refined as rotating group:
 O00B(H1), O00D(H4), O012(H012), O013(H013), O3(H3A), O2(H2), O01U(H01R),
 O0(H0A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44146
_shelx_fab_checksum              78006
_olex2_submission_special_instructions 'No special instructions were received'