Redox-inactive ions control the redox-activity of molecular vanadium oxides
Greiner, Simon; Schwarz, Benjamin; Ringenberg, Mark; Dürr, Maximilian; Ivanovic-Burmazovic, Ivana; Fichtner, Maximilian; Anjass, Montaha; Streb, Carsten; Chemical Science 11 (2020) 4450–4455; doi:10.1039/D0SC01401J

data_1557747
_publ_section_title
;
 Redox-inactive ions control the redox-activity of molecular vanadium
 oxides
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4450
_journal_page_last               4455
_journal_paper_doi               10.1039/D0SC01401J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety
'C9 H21 Ca2 N3 O35 V12, Cl, C16 H36 N, C16 H32 N, C3 H7 N O'
_chemical_formula_sum            'C44 H96 Ca2 Cl N6 O36 V12'
_chemical_formula_weight         2012.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3952(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6954(5)
_cell_length_b                   29.2218(14)
_cell_length_c                   28.2691(15)
_cell_measurement_reflns_used    9416
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.21
_cell_volume                     8796.1(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.97
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            204730
_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         26.398
_diffrn_reflns_theta_min         2.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0785 before and 0.0655 after correction. The Ratio of minimum to maximum transmission is 0.9195. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             4092
_exptl_crystal_recrystallization_method DMF/Acetone
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         18025
_refine_ls_number_restraints     462
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0815
_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^)+(0.0323P)^2^+86.5979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15013
_reflns_number_total             18025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01401j2.cif
_cod_data_source_block           bs17021_0m
_cod_depositor_comments
;Adding full bibliography for 1557747.cif.

 Adding full bibliography for 1557747.cif.
;
_cod_original_cell_volume        8796.0(8)
_cod_database_code               1557747
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Others
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C35(0.5) H35(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) H46(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5)
 Fixed Uiso: H1A(0.071) H1B(0.071) H2A(0.079) H2B(0.079) H3A(0.067) H3B(0.067)
 H4A(0.086) H4B(0.086) H5A(0.095) H5B(0.095) H6A(0.071) H6B(0.071) H7(0.132)
 H8A(0.082) H8B(0.082) H9A(0.092) H9B(0.092) H10A(0.11) H10B(0.11) H11A(0.073)
 H11B(0.073) H12A(0.079) H12B(0.079) H13A(0.108) H13B(0.108) H14A(0.122)
 H14B(0.122) H15A(0.127) H15B(0.127) H16A(0.137) H16B(0.137) H17A(0.17)
 H17B(0.17) H17C(0.17) H18A(0.071) H18B(0.071) H19A(0.12) H19B(0.12)
 H21A(0.127) H21B(0.127) H22A(0.09) H22B(0.09) H23(0.188) H24A(0.202)
 H24B(0.202) H24C(0.202) H25A(0.125) H25B(0.125) H26A(0.288) H26B(0.288)
 H26C(0.288) H27A(0.3) H27B(0.3) H27C(0.3) H28A(0.214) H28B(0.214) H28C(0.214)
 H29A(0.213) H29B(0.213) H29C(0.213) H30A(0.177) H30B(0.177) H30C(0.177)
 H31A(0.131) H31B(0.131) H32A(0.229) H32B(0.229) H32C(0.229) H33A(0.159)
 H33B(0.159) H33C(0.159) H34A(0.239) H34B(0.239) H34C(0.239) H35(0.085)
 H36(0.156) H38A(0.305) H38B(0.305) H38C(0.305) H39A(0.299) H39B(0.299)
 H39C(0.299) H40A(0.273) H40B(0.273) H40C(0.273) H41A(0.193) H41B(0.193)
 H41C(0.193) H42A(0.145) H42B(0.145) H43A(0.374) H43B(0.374) H43C(0.374)
 H44A(0.175) H44B(0.175) H44C(0.175) H45A(0.253) H45B(0.253) H45C(0.253)
 H46(0.088) H47A(0.214) H47B(0.214) H47C(0.214) H49A(0.202) H49B(0.202)
 H50A(0.302) H50B(0.302) H50C(0.302)
 Fixed X: H1A(-0.1321) H1B(-0.0061) H2A(0.0098) H2B(0.0699) H3A(-0.096) H3B(-
 0.227) H4A(-0.1218) H4B(-0.2303) H5A(-0.0235) H5B(0.1033) H6A(-0.1186) H6B(-
 0.1678) H7(0.3788) H8A(-0.2925) H8B(-0.3435) H9A(0.1033) H9B(0.1593) H10A(-
 0.3088) H10B(-0.3526) H11A(-0.0083) H11B(-0.0731) H12A(0.1796) H12B(0.1184)
 H13A(-0.2095) H13B(-0.2719) H14A(-0.259) H14B(-0.3671) H15A(-0.0269)
 H15B(0.0955) H16A(0.4338) H16B(0.3206) H17A(-0.4169) H17B(-0.277) H17C(-
 0.3647) H18A(0.0423) H18B(0.1761) H19A(0.3177) H19B(0.2518) H21A(-0.2021)
 H21B(-0.1339) H22A(0.0947) H22B(0.2172) H23(0.4401) H24A(0.3878) H24B(0.4255)
 H24C(0.3317) H25A(0.227) H25B(0.2786) H26A(0.3615) H26B(0.3322) H26C(0.473)
 H27A(0.4423) H27B(0.2992) H27C(0.4007) H28A(-0.4963) H28B(-0.54) H28C(-0.523)
 H29A(0.5151) H29B(0.376) H29C(0.3976) H30A(0.2233) H30B(0.3494) H30C(0.3386)
 H31A(0.1895) H31B(0.3129) H32A(0.4233) H32B(0.4098) H32C(0.5415) H33A(-0.5504)
 H33B(-0.6939) H33C(-0.6536) H34A(0.149) H34B(0.0906) H34C(0.2132) H35(-0.5838)
 H36(0.2381) H38A(-0.3532) H38B(-0.413) H38C(-0.4251) H39A(0.0339) H39B(-
 0.0014) H39C(0.0164) H40A(0.2952) H40B(0.1576) H40C(0.2459) H41A(-0.5462)
 H41B(-0.587) H41C(-0.6918) H42A(-0.0578) H42B(-0.1749) H43A(0.3483)
 H43B(0.4776) H43C(0.4566) H44A(-0.6495) H44B(-0.5267) H44C(-0.5194) H45A(-
 0.2751) H45B(-0.2192) H45C(-0.1538) H46(-0.6335) H47A(-0.5893) H47B(-0.5582)
 H47C(-0.7007) H49A(0.0041) H49B(0.0897) H50A(-0.1589) H50B(-0.0342) H50C(-
 0.0631)
 Fixed Y: H1A(0.6513) H1B(0.6784) H2A(0.7391) H2B(0.6893) H3A(0.7495)
 H3B(0.7242) H4A(0.7952) H4B(0.7635) H5A(0.604) H5B(0.6324) H6A(0.6493)
 H6B(0.6989) H7(0.8772) H8A(0.6422) H8B(0.6906) H9A(0.7611) H9B(0.7106)
 H10A(0.611) H10B(0.6594) H11A(1.0094) H11B(1.0013) H12A(1.0012) H12B(0.9995)
 H13A(1.008) H13B(0.9947) H14A(0.8182) H14B(0.7861) H15A(0.5814) H15B(0.6114)
 H16A(1.0222) H16B(0.9869) H17A(0.8575) H17B(0.8678) H17C(0.8334) H18A(1.1095)
 H18B(1.1055) H19A(1.0592) H19B(1.0618) H21A(1.0649) H21B(1.0756) H22A(1.057)
 H22B(1.0414) H23(0.7031) H24A(0.7388) H24B(0.7728) H24C(0.7896) H25A(0.7714)
 H25B(0.7202) H26A(0.7243) H26B(0.6723) H26C(0.6913) H27A(0.847) H27B(0.8522)
 H27C(0.89) H28A(0.6027) H28B(0.6525) H28C(0.6124) H29A(0.6222) H29B(0.6163)
 H29C(0.6214) H30A(1.0757) H30B(1.0599) H30C(1.1105) H31A(1.1293) H31B(1.1117)
 H32A(0.7669) H32B(0.7714) H32C(0.782) H33A(0.8405) H33B(0.8557) H33C(0.8236)
 H34A(0.5353) H34B(0.5323) H34C(0.5626) H35(0.9132) H36(0.6638) H38A(1.066)
 H38B(1.0556) H38C(1.0187) H39A(0.6804) H39B(0.6485) H39C(0.6264) H40A(0.603)
 H40B(0.6012) H40C(0.6446) H41A(0.9358) H41B(0.9582) H41C(0.9403) H42A(1.0887)
 H42B(1.0983) H43A(0.9598) H43B(0.9568) H43C(0.9966) H44A(0.9407) H44B(0.9507)
 H44C(0.9163) H45A(1.0409) H45B(1.0694) H45C(1.0226) H46(0.8235) H47A(0.8704)
 H47B(0.9234) H47C(0.9061) H49A(1.0905) H49B(1.0462) H50A(1.0414) H50B(1.0411)
 H50C(0.9993)
 Fixed Z: H1A(-0.0391) H1B(-0.0466) H2A(0.0642) H2B(0.0619) H3A(-0.0361) H3B(-
 0.0324) H4A(0.0269) H4B(0.0445) H5A(0.0177) H5B(0.0134) H6A(0.0635)
 H6B(0.0765) H7(0.3366) H8A(0.0049) H8B(0.0218) H9A(-0.0032) H9B(-0.008)
 H10A(0.0822) H10B(0.1008) H11A(0.1959) H11B(0.2438) H12A(0.2418) H12B(0.2911)
 H13A(0.1465) H13B(0.1936) H14A(-0.0405) H14B(-0.0235) H15A(-0.0625) H15B(-
 0.0685) H16A(0.334) H16B(0.3371) H17A(-0.0031) H17B(0.0197) H17C(0.0457)
 H18A(0.2053) H18B(0.2352) H19A(0.2704) H19B(0.3188) H21A(0.2277) H21B(0.1809)
 H22A(0.1511) H22B(0.184) H23(0.2901) H24A(0.006) H24B(0.0494) H24C(0.0054)
 H25A(0.0711) H25B(0.0689) H26A(0.1748) H26B(0.1599) H26C(0.162) H27A(0.4505)
 H27B(0.4289) H27C(0.4176) H28A(0.036) H28B(0.0513) H28C(0.0898) H29A(0.2341)
 H29B(0.2086) H29C(0.2652) H30A(0.0827) H30B(0.1133) H30C(0.0918) H31A(0.1411)
 H31B(0.1718) H32A(0.3603) H32B(0.4161) H32C(0.3958) H33A(0.0991) H33B(0.0879)
 H33C(0.1327) H34A(-0.0615) H34B(-0.0116) H34C(-0.0165) H35(0.2088) H36(0.3832)
 H38A(0.131) H38B(0.1797) H38C(0.1376) H39A(0.4125) H39B(0.4554) H39C(0.4047)
 H40A(0.4799) H40B(0.4977) H40C(0.5099) H41A(0.0975) H41B(0.1454) H41C(0.1055)
 H42A(0.3851) H42B(0.3477) H43A(0.2638) H43B(0.2971) H43C(0.2583) H44A(0.1852)
 H44B(0.1586) H44C(0.2028) H45A(0.3716) H45B(0.4171) H45C(0.4034) H46(0.134)
 H47A(0.0754) H47B(0.0845) H47C(0.0805) H49A(0.3784) H49B(0.374) H50A(0.4048)
 H50B(0.4408) H50C(0.4048)
;
_olex2_submission_special_instructions 'No special instructions were received'