A benzene-bridged divanadium complex-early transition metal catalyst for alkene alkylarylation with PhI(O<sub>2</sub>CR)<sub>2</sub><i>via</i> decarboxylation.
Zhang, Lei; Zhou, Hongfei; Bai, Shaokun; Li, Shaodan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3201–3206; doi:10.1039/d0dt04295a

data_7706554
_publ_section_title
;
 A benzene-bridged divanadium complex-early transition metal catalyst for
 alkene alkylarylation with PhI(O<sub>2</sub>CR)<sub>2</sub><i>via</i>
 decarboxylation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3201
_journal_page_last               3206
_journal_paper_doi               10.1039/d0dt04295a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C64 H88 N4 V2'
_chemical_formula_sum            'C64 H88 N4 V2'
_chemical_formula_weight         1015.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2021-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.363(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2394(4)
_cell_length_b                   13.5889(3)
_cell_length_c                   15.0927(4)
_cell_measurement_reflns_used    5643
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7590
_cell_measurement_theta_min      4.9600
_cell_volume                     2802.12(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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    -70.00  46.00   1.00    1.65    --  -41.49   0.00-120.00  116
  2  \w     32.00  78.00   1.00    1.65    --   41.49-125.00  60.00   46
  3  \w     15.00  60.00   1.00    1.65    --   41.49 -99.00-180.00   45
  4  \w     32.00  86.00   1.00    3.00    --  104.69 -45.00-180.00   54
  5  \w     79.00 175.00   1.00    3.00    --  104.69  61.00 -30.00   96
  6  \w     94.00 120.00   1.00    3.00    --  104.69 125.00 -90.00   26
  7  \w     94.00 178.00   1.00    3.00    --  104.69 125.00-120.00   84
  8  \w     94.00 131.00   1.00    3.00    --  104.69 -45.00-180.00   37
  9  \w     34.00  59.00   1.00    3.00    --  104.69-125.00  90.00   25
 10  \w     87.00 112.00   1.00    3.00    --  104.69-125.00  90.00   25
 11  \w     56.00 107.00   1.00    3.00    --  104.69 -94.00 -90.00   51
 12  \w     30.00 105.00   1.00    3.00    --  104.69 -94.00-180.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0548250000
_diffrn_orient_matrix_UB_12      0.0882723000
_diffrn_orient_matrix_UB_13      -0.0259814000
_diffrn_orient_matrix_UB_21      -0.0455029000
_diffrn_orient_matrix_UB_22      0.0682091000
_diffrn_orient_matrix_UB_23      0.0582433000
_diffrn_orient_matrix_UB_31      0.0873564000
_diffrn_orient_matrix_UB_32      -0.0198816000
_diffrn_orient_matrix_UB_33      0.0852094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11321
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.969
_diffrn_reflns_theta_min         3.771
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5383
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0385P)^2^+2.8605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4862
_reflns_number_total             5383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04295a2.cif
_cod_data_source_block           20190410a
_cod_depositor_comments          'Adding full bibliography for 7706554.cif.'
_cod_database_code               7706554
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Cl1V1Si1
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.576
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 C33-H33 = C34-H34 = C35-H35
 0.93 with sigma of 0.02
 C12-C13 \\sim C12-C14 \\sim C12-C13A \\sim C12-C14A
 with sigma of 0.02
3. Rigid bond restraints
 C7, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim C12: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C14) = Uanis(C13)
5. Others
 Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C12(H12A), C15(H15), C24(H24), C27(H27)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F),
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              79282
_shelx_hkl_checksum              31286
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.764