Nuclear-spin-pattern control of electron-spin dynamics in a series of V(iv) complexes
Jackson, Cassidy E.; Lin, Chun-Yi; Johnson, Spencer H.; van Tol, Johan; Zadrozny, Joseph M.; Chemical Science  (2019) –; doi:10.1039/C9SC02899D

data_1552145
_publ_section_title
;
 Nuclear-spin-pattern control of electron-spin dynamics in a series of
 V(iv) complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02899D
_journal_year                    2019
_chemical_formula_moiety         'Br12 C18 O6 V, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br12 N2 O6 V'
_chemical_formula_weight         1694.63
_chemical_name_common            (n-Bu3NH)2[V(C6Br4O2)3]
_chemical_name_systematic
'tris(tetrabromocatecholato)vanadate(IV) bis-tri-n-butylammonium'
_chemical_properties_physical    Air-sensitive,Heat-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-07 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                83.93(3)
_cell_angle_beta                 89.04(2)
_cell_angle_gamma                84.219(19)
_cell_formula_units_Z            4
_cell_length_a                   12.039(5)
_cell_length_b                   12.432(6)
_cell_length_c                   37.11(2)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      26.484
_cell_measurement_theta_min      2.277
_cell_volume                     5495(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      145.03
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.958
_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       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            46089
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_min         3.783
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    8.950
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1344 before and 0.0554 after correction. The Ratio of minimum to maximum transmission is 0.4797. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             51
_exptl_crystal_recrystallization_method layering
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         21824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0653
_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^)+83.8435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17019
_reflns_number_total             21824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02899d2.cif
_cod_data_source_block           jz25_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1552145
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N014(H014), N01G(H01G), N01Q(H01Q), N025(H025)
3.b Secondary CH2 refined with riding coordinates:
 C01X(H01A,H01B), C021(H02I,H02J), C022(H02,H), C026(H02K,H02L), C029(H02M,
 H02N), C02C(H02R,H02S), C02E(H02T,H02U), C02F(H0AA,HA), C02G(H3AA,HB),
 C02H(H1BA,HC), C02I(H02A,H02B), C02J(H02V,H02W), C02K(H4AA,HD), C02L(H02X,
 H02Y), C02N(H02C,H02D), C02O(H6AA,HG), C02P(H7AA,HH), C02Q(H2BA,HI), C02S(H3BA,
 HL), C02T(H02E,H02F), C02U(H8AA,HM), C02V(H9AA,HN), C02W(H4BA,HO), C02Y(H02G,
 H02H), C02Z(H0BA,HR), C030(H03A,H03B), C031(H03Z,HS), C032(H03O,H03P),
 C033(H03,HT), C034(H6BA,HU), C036(H7BA,HV), C037(H03C,H03D), C038(H8BA,HW),
 C039(H03E,H03F), C03A(H03G,H03H), C1(H1AA,H1AB), C1(H1BC,H1BD)
3.c Idealised Me refined as rotating group:
 C02B(H02O,H02P,H02Q), C02M(H5AA,HE,HF), C02R(H02Z,HJ,HK), C02X(H5BA,HP,HQ),
 C035(H03T,H03U,H03V), C03B(H03I,H03J,H03K), C03C(H03L,H03M,H03N), C03D(H9BA,HX,
 HY), C03E(H0CA,HZ,H1CA), C03G(H03W,H03X,H03Y), C03H(H03Q,H03R,H03S), C2(H2A,
 H2B,H2C), C2A(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              92594
_olex2_submission_special_instructions 'No special instructions were received'