Supramolecular bimetallic vanadium(V) complex driven by hydrogen bonding and O∙∙∙O chalcogen bonding interaction: Oxidation of cyclohexane and its application toward C H bond activation
Kurbah, Sunshine Dominic; Clovis, Ndege Simisi; Inorganica Chimica Acta 511 (2020) 119837–; doi:10.1016/j.ica.2020.119837

data_1564180
_publ_section_title
;
 Supramolecular bimetallic vanadium(V) complex driven by hydrogen bonding
 and O&#x2219;&#x2219;&#x2219;O chalcogen bonding interaction: Oxidation
 of cyclohexane and its application toward C H bond activation
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119837
_journal_paper_doi               10.1016/j.ica.2020.119837
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C30 H35 N5 Na2 O15 V2, H2 O'
_chemical_formula_sum            'C30 H37 N5 Na2 O16 V2'
_chemical_formula_weight         871.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                98.623(9)
_cell_angle_beta                 91.246(6)
_cell_angle_gamma                104.582(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3309(6)
_cell_length_b                   11.9489(19)
_cell_length_c                   19.6741(15)
_cell_measurement_reflns_used    2587
_cell_measurement_temperature    296.08(11)
_cell_measurement_theta_max      28.8120
_cell_measurement_theta_min      3.8920
_cell_volume                     1870.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.08(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -25.00  24.00   1.00    2.27    --  -17.59 -99.00  90.00   49
  2  \w     46.00  88.00   1.00    2.27    --   19.93-178.00 120.00   42
  3  \w    -47.00  44.00   1.00    2.27    --   19.93 -37.00 150.00   91
  4  \w    -90.00 -40.00   1.00    2.27    --  -17.59 149.00-141.00   50
  5  \w    -25.00  90.00   1.00    2.27    --   19.93   0.00-180.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0074008000
_diffrn_orient_matrix_UB_12      -0.0063660000
_diffrn_orient_matrix_UB_13      0.0351507000
_diffrn_orient_matrix_UB_21      0.0159739000
_diffrn_orient_matrix_UB_22      0.0616589000
_diffrn_orient_matrix_UB_23      0.0092848000
_diffrn_orient_matrix_UB_31      -0.0863692000
_diffrn_orient_matrix_UB_32      -0.0044140000
_diffrn_orient_matrix_UB_33      -0.0036134000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10696
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       needle
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.916
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.512
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.512
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.1357
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3849
_refine_ls_wR_factor_ref         0.4016
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5028
_reflns_number_total             6537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119837.cif
_cod_data_source_block           sdk-39a
_cod_database_code               1564180
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B)
2.b Rotating group:
 O13(H13A,H13B), O9(H9A,H9B), O15(H15A,H15B), O11(H11A,H11B)
2.c Secondary CH2 refined with riding coordinates:
 C15(H15C,H15D), C14(H14A,H14B), C13(H13C,H13D)
2.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C21(H21), C3(H3), C26(H26), C23(H23), C20(H20), C6(H6),
 C9(H9), C4(H4), C8(H8), C25(H25), C24(H24), C7(H7), C28(H28)
2.e Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              1439
_shelx_hkl_checksum              95405