Counterion Influence on Dynamic Spin Properties in a V(IV) Complex
Lin, Chun-Yi; Ngendahimana, Thacien; Eaton, Gareth; Eaton, Sandra S.; Zadrozny, Joseph; Chemical Science  (2019) –; doi:10.1039/C8SC04122A

data_1550054
_publ_section_title
;
 Counterion Influence on Dynamic Spin Properties in a V(IV) Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04122A
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C18 H12 O6 V, 2(C18 H40 N)'
_chemical_formula_sum            'C54 H92 N2 O6 V'
_chemical_formula_weight         916.23
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.546(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.013(5)
_cell_length_b                   23.356(6)
_cell_length_c                   15.400(3)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.713
_cell_measurement_theta_min      2.503
_cell_volume                     5568(2)
_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)'
_diffrn_ambient_temperature      100.37
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49029
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.7081
_exptl_absorpt_correction_T_min  0.5003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0969 before and 0.0719 after correction. The Ratio of minimum to maximum transmission is 0.7065. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, hexanes'
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.536
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 4010 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.090(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         11209
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0293P)^2^+27.7042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                9707
_reflns_number_total             11209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04122a2.cif
_cod_data_source_block           jz16_0m
_cod_database_code               1550054
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.04) H3(0.04) H4(0.04) H5(0.04) H8(0.033) H9(0.041)
 H10(0.047) H11(0.04) H14(0.03) H15(0.038) H16(0.045) H17(0.043) H1(0.027)
 H19A(0.029) H19B(0.029) H20A(0.034) H20B(0.034) H21A(0.042) H21B(0.042)
 H22A(0.044) H22B(0.044) H23A(0.063) H23B(0.063) H24A(0.095) H24B(0.095)
 H24C(0.095) H25A(0.029) H25B(0.029) H26A(0.031) H26B(0.031) H27A(0.037)
 H27B(0.037) H28A(0.037) H28B(0.037) H29A(0.047) H29B(0.047) H30A(0.055)
 H30B(0.055) H30C(0.055) H31A(0.033) H31B(0.033) H32A(0.038) H32B(0.038)
 H33A(0.042) H33B(0.042) H34A(0.043) H34B(0.043) H35A(0.051) H35B(0.051)
 H36A(0.088) H36B(0.088) H36C(0.088) H2(0.027) H37A(0.033) H37B(0.033)
 H38A(0.041) H38B(0.041) H39A(0.037) H39B(0.037) H40A(0.045) H40B(0.045)
 H41A(0.053) H41B(0.053) H42A(0.085) H42B(0.085) H42C(0.085) H43A(0.031)
 H43B(0.031) H44A(0.036) H44B(0.036) H45A(0.043) H45B(0.043) H46A(0.051)
 H46B(0.051) H46C(0.051) H46D(0.051) H49A(0.03) H49B(0.03) H50A(0.032)
 H50B(0.032) H51A(0.04) H51B(0.04) H52A(0.041) H52B(0.041) H53A(0.047)
 H53B(0.047) H54A(0.058) H54B(0.058) H54C(0.058) H5A(0.04) H4A(0.04) H3A(0.04)
 H2AA(0.04) H47A(0.058) H47B(0.058) H48A(0.073) H48B(0.073) H48C(0.073)
 H47C(0.058) H47D(0.058) H48D(0.073) H48E(0.073) H48F(0.073)
 Fixed X: H2A(-0.458134) H3(-0.312385) H4(-0.202713) H5(-0.236619) H8(-
 0.566795) H9(-0.706312) H10(-0.820879) H11(-0.795778) H14(-0.555655) H15(-
 0.543036) H16(-0.518228) H17(-0.502316) H1(-0.479954) H19A(-0.390778) H19B(-
 0.486364) H20A(-0.449011) H20B(-0.359748) H21A(-0.352216) H21B(-0.388806)
 H22A(-0.230395) H22B(-0.267162) H23A(-0.209049) H23B(-0.246312) H24A(-
 0.128307) H24B(-0.094012) H24C(-0.09165) H25A(-0.37396) H25B(-0.408009) H26A(-
 0.279606) H26B(-0.321634) H27A(-0.264747) H27B(-0.239108) H28A(-0.127996)
 H28B(-0.155593) H29A(-0.09506) H29B(-0.108608) H30A(0.039841) H30B(0.008784)
 H30C(0.023148) H31A(-0.529087) H31B(-0.544471) H32A(-0.619142) H32B(-0.626113)
 H33A(-0.699619) H33B(-0.697844) H34A(-0.782484) H34B(-0.78713) H35A(-0.869152)
 H35B(-0.861626) H36A(-0.998789) H36B(-0.946721) H36C(-0.951358) H2(-0.707222)
 H37A(-0.70028) H37B(-0.800893) H38A(-0.835559) H38B(-0.735613) H39A(-0.717368)
 H39B(-0.819053) H40A(-0.743243) H40B(-0.845143) H41A(-0.739856) H41B(-0.84072)
 H42A(-0.875124) H42B(-0.77486) H42C(-0.815104) H43A(-0.80996) H43B(-0.85313)
 H44A(-0.916131) H44B(-0.859291) H45A(-0.975854) H45B(-1.011492) H46A(-0.87869)
 H46B(-0.916973) H46C(-0.929385) H46D(-0.876742) H49A(-0.720467) H49B(-
 0.633967) H50A(-0.735775) H50B(-0.65977) H51A(-0.555673) H51B(-0.627498) H52A(-
 0.600362) H52B(-0.666776) H53A(-0.481971) H53B(-0.543312) H54A(-0.598714)
 H54B(-0.495826) H54C(-0.539761) H5A(-0.224146) H4A(-0.167019) H3A(-0.259635)
 H2AA(-0.409623) H47A(-1.048924) H47B(-1.010101) H48A(-0.998131) H48B(-
 0.959056) H48C(-0.901979) H47C(-1.064704) H47D(-1.010511) H48D(-1.054663)
 H48E(-1.023206) H48F(-0.953656)
 Fixed Y: H2A(-0.633587) H3(-0.633516) H4(-0.620243) H5(-0.615615) H8(-
 0.433657) H9(-0.39819) H10(-0.459507) H11(-0.559401) H14(-0.816212) H15(-
 0.852638) H16(-0.790938) H17(-0.691453) H1(-0.584002) H19A(-0.607116) H19B(-
 0.597611) H20A(-0.51377) H20B(-0.509357) H21A(-0.545105) H21B(-0.604002) H22A(-
 0.552594) H22B(-0.61044) H23A(-0.59943) H23B(-0.657467) H24A(-0.662519) H24B(-
 0.659038) H24C(-0.603374) H25A(-0.486232) H25B(-0.512195) H26A(-0.563127)
 H26B(-0.59774) H27A(-0.534598) H27B(-0.489369) H28A(-0.550256) H28B(-0.598182)
 H29A(-0.488023) H29B(-0.542417) H30A(-0.530578) H30B(-0.589396) H30C(-
 0.533906) H31A(-0.485165) H31B(-0.489387) H32A(-0.562346) H32B(-0.575763)
 H33A(-0.486137) H33B(-0.477345) H34A(-0.56267) H34B(-0.568392) H35A(-0.483073)
 H35B(-0.47457) H36A(-0.514323) H36B(-0.557515) H36C(-0.568874) H2(-0.667233)
 H37A(-0.760653) H37B(-0.767117) H38A(-0.689604) H38B(-0.674384) H39A(-
 0.763785) H39B(-0.77499) H40A(-0.682303) H40B(-0.688864) H41A(-0.766959) H41B(-
 0.776921) H42A(-0.696008) H42B(-0.681425) H42C(-0.737214) H43A(-0.644025)
 H43B(-0.654105) H44A(-0.738381) H44B(-0.740374) H45A(-0.647686) H45B(-
 0.706443) H46A(-0.639759) H46B(-0.697318) H46C(-0.694764) H46D(-0.641493)
 H49A(-0.76505) H49B(-0.738362) H50A(-0.688464) H50B(-0.653387) H51A(-0.717373)
 H51B(-0.761846) H52A(-0.65334) H52B(-0.700883) H53A(-0.710187) H53B(-0.763453)
 H54A(-0.715094) H54B(-0.719646) H54C(-0.660686) H5A(-0.617715) H4A(-0.616547)
 H3A(-0.632063) H2AA(-0.633416) H47A(-0.649856) H47B(-0.592048) H48A(-0.582415)
 H48B(-0.645437) H48C(-0.595907) H47C(-0.644778) H47D(-0.591376) H48D(-
 0.566451) H48E(-0.626289) H48F(-0.579871)
 Fixed Z: H2A(-0.728077) H3(-0.634512) H4(-0.431425) H5(-0.310734) H8(-
 0.503308) H9(-0.650085) H10(-0.786996) H11(-0.775619) H14(-0.480943) H15(-
 0.327604) H16(-0.187825) H17(-0.197188) H1(-0.26325) H19A(-0.069663) H19B(-
 0.121779) H20A(-0.019407) H20B(0.01059) H21A(0.170858) H21B(0.098991)
 H22A(0.193713) H22B(0.119149) H23A(0.348066) H23B(0.273193) H24A(0.286334)
 H24B(0.415869) H24C(0.3575) H25A(-0.144343) H25B(-0.265532) H26A(-0.036741)
 H26B(-0.154947) H27A(-0.203615) H27B(-0.10639) H28A(0.045799) H28B(-0.04852)
 H29A(-0.046613) H29B(-0.12073) H30A(0.04381) H30B(0.05836) H30C(0.130839)
 H31A(-0.213956) H31B(-0.330732) H32A(-0.271755) H32B(-0.379874) H33A(-0.4669)
 H33B(-0.362169) H34A(-0.4239) H34B(-0.531515) H35A(-0.615902) H35B(-0.506096)
 H36A(-0.670521) H36B(-0.561096) H36C(-0.667749) H2(-0.715766) H37A(-0.643282)
 H37B(-0.757965) H38A(-0.701004) H38B(-0.595146) H39A(-0.5027) H39B(-0.605642)
 H40A(-0.439445) H40B(-0.547028) H41A(-0.353543) H41B(-0.463642) H42A(-
 0.412256) H42B(-0.307467) H42C(-0.299843) H43A(-0.906503) H43B(-0.85348) H44A(-
 0.955671) H44B(-0.99014) H45A(-1.070348) H45B(-1.142714) H46A(-1.09987) H46B(-
 1.174898) H46C(-1.19463) H46D(-1.104068) H49A(-0.834708) H49B(-0.715224) H50A(-
 0.945918) H50B(-0.829098) H51A(-0.78221) H51B(-0.88026) H52A(-0.935185) H52B(-
 1.030043) H53A(-0.86435) H53B(-0.942162) H54A(-1.115104) H54B(-1.027511) H54C(-
 1.038852) H5A(-0.249489) H4A(-0.344587) H3A(-0.546422) H2AA(-0.668908) H47A(-
 1.326435) H47B(-1.251167) H48A(-1.3869) H48B(-1.36181) H48C(-1.265973) H47C(-
 1.286875) H47D(-1.201392) H48D(-1.379832) H48E(-1.39034) H48F(-1.295272)
;
_olex2_submission_special_instructions 'No special instructions were received'