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_7706981
_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         'C9 H30 Cr N6, 3(Cl), 2(H2 O), 0.5(C2 H6 O)'
_chemical_formula_sum            'C9 H30 Cl3 Cr N6 O0.12'
_chemical_formula_weight         382.74
_chemical_name_systematic        Tris(1,3-propanediamine)Chromium(III)Chloride
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-03-20
_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                 121.059(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.4948(19)
_cell_length_b                   12.0595(7)
_cell_length_c                   14.7903(8)
_cell_measurement_reflns_used    9712
_cell_measurement_temperature    154.01
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      2.74
_cell_volume                     4353.8(5)
_computing_cell_refinement       'SAINT V8.38A (?, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      154.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.839
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.790
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.129
_diffrn_reflns_theta_min         1.607
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.8304.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water, Ethanol'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.217
_refine_ls_abs_structure_details
;
 Flack x determined using 4295 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         12060
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0853P)^2^+42.3121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2117
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.741
_reflns_number_gt                10038
_reflns_number_total             12060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00066g2.cif
_cod_data_source_block           jz88_0ma_b
_cod_depositor_comments
'Adding full bibliography for 7706979--7706982.cif.'
_cod_database_code               7706981
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(6)
 0.48(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C7AC-C2
 1.54 with sigma of 0.02
 O1A-C2
 1.45 with sigma of 0.01
 C2A-C7AD
 1.55 with sigma of 0.02
 O1B-C2A \\sim O1A-C2
 with sigma of 0.01
 C7AC-C2 \\sim C7AD-C2A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C7AC \\sim C2 \\sim O1A: within 1.7A with sigma of 0.03 and sigma for terminal
atoms of 0.07 within 1.7A
O1A \\sim C2 \\sim C7AC: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
5. Others
 Sof(Cl)=1-FVAR(1)
 Sof(Cl08)=FVAR(1)
 Sof(N0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(C0AA)=Sof(H0AC)=
 Sof(H0AD)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(N1AA)=Sof(H1AC)=Sof(H1AD)=1-FVAR(2)
 Sof(N00E)=Sof(H00E)=Sof(H00F)=Sof(N00H)=Sof(H00G)=Sof(H00H)=Sof(C00W)=
 Sof(H00M)=Sof(H00N)=Sof(C00X)=Sof(H00O)=Sof(H00P)=Sof(C019)=Sof(H01C)=
 Sof(H01D)=FVAR(2)
 Sof(N00V)=Sof(H00Q)=Sof(H00R)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(C00C)=
 Sof(H00S)=Sof(H00T)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(N2AA)=Sof(H2AC)=
 Sof(H2AD)=1-FVAR(3)
 Sof(C00B)=Sof(H00A)=Sof(H00B)=Sof(N00D)=Sof(H00C)=Sof(H00D)=Sof(N00U)=
 Sof(H00I)=Sof(H00J)=Sof(C00V)=Sof(H00K)=Sof(H00L)=Sof(C010)=Sof(H01A)=
 Sof(H01B)=FVAR(3)
 Sof(H00W)=Sof(H00X)=Sof(C00U)=Sof(H8)=Sof(HO)=Sof(C6AB)=Sof(H6AC)=Sof(H6AD)=
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(N1)=Sof(H1C)=Sof(H1D)=1-FVAR(4)
 Sof(H00U)=Sof(H00V)=Sof(N00J)=Sof(H00)=Sof(HB)=Sof(C00T)=Sof(H6)=Sof(HM)=
 Sof(C012)=Sof(H01E)=Sof(H01F)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=FVAR(4)
 Sof(HD)=Sof(HE)=Sof(C00N)=Sof(H9)=Sof(HP)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(N00R)=Sof(H10)=Sof(HQ)=1-FVAR(5)
 Sof(H1)=Sof(HC)=Sof(C00M)=Sof(H3)=Sof(HG)=Sof(N00Q)=Sof(H4)=Sof(HK)=Sof(C014)=
 Sof(H01G)=Sof(H01H)=Sof(C016)=Sof(H01I)=Sof(H01J)=FVAR(5)
 Sof(O1B)=Sof(H1BA)=Sof(C2A)=Sof(H2AF)=Sof(H2AE)=Sof(C7AD)=Sof(H7AD)=Sof(H7AE)=
 Sof(H7AF)=1-FVAR(6)
 Sof(O1A)=Sof(H1AE)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C7AC)=Sof(H7AA)=Sof(H7AB)=
 Sof(H7AC)=FVAR(6)
 Fixed Sof: O00O(0.5) H12(0.5) HI(0.5) O00P(0.5) H13(0.5) HJ(0.5)
6.a Free rotating group:
 O00N(H11,HH), O00O(H12,HI), O00P(H13,HJ), O0AA(H0AE,H0AF), O00B(H14,HR)
6.b Secondary CH2 refined with riding coordinates:
 N009(H00U,H00V), N009(H00W,H00X), C00B(H00A,H00B), N00C(H00Y,H), N00D(H00C,
 H00D), N00E(H00E,H00F), N00H(H00G,H00H), N00I(H00Z,HA), N00J(H00,HB), N00K(H1,
 HC), N00K(HD,HE), C00L(H2,HF), C00M(H3,HG), N00Q(H4,HK), C00R(H5,HL), C00T(H6,
 HM), N00U(H00I,H00J), C00V(H00K,H00L), C00W(H00M,H00N), C00X(H00O,H00P),
 C00Z(H7,HN), C010(H01A,H01B), C012(H01E,H01F), C014(H01G,H01H), C016(H01I,
 H01J), C019(H01C,H01D), C6AA(H6AA,H6AB), N0AA(H0AA,H0AB), C0(H0A,H0B),
 C0AA(H0AC,H0AD), C1AA(H1AA,H1AB), N1AA(H1AC,H1AD), N00V(H00Q,H00R), C5AA(H5AA,
 H5AB), C00C(H00S,H00T), C2AA(H2AA,H2AB), N2AA(H2AC,H2AD), N3AA(H3AA,H3AB),
 C3(H3A,H3B), C3AA(H3AC,H3AD), C4AA(H4AA,H4AB), N4AA(H4AC,H4AD), C2(H2A,H2B),
 C00U(H8,HO), C6AB(H6AC,H6AD), C1(H1A,H1B), N1(H1C,H1D), C00N(H9,HP), C4(H4A,
 H4B), C5(H5A,H5B), N00R(H10,HQ), C2A(H2AF,H2AE)
6.c Idealised Me refined as rotating group:
 C7AC(H7AA,H7AB,H7AC), C7AD(H7AD,H7AE,H7AF)
6.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1AE), O1B(H1BA)
;
_shelx_res_checksum              49850
_olex2_submission_special_instructions 'No special instructions were received'