Crystal structure of heptakis(2,6-dimethylphenyl isocyanide-κ<i>C</i>)vanadium(I) iodide
Minyaev, Mikhail E.; Ellis, John E.; Acta Crystallographica Section E 71 (2015) 431–434; doi:10.1107/S2056989015006015

data_2240550
_publ_section_title
;
 Crystal structure of heptakis(2,6-dimethylphenyl
 isocyanide-\k<i>C</i>)vanadium(I) iodide
;
_journal_coeditor_code           WM5140
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              431
_journal_page_last               434
_journal_paper_doi               10.1107/S2056989015006015
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[V (C9 H9 N)7] I'
_chemical_formula_moiety         'C63 H63 N7 V, I'
_chemical_formula_sum            'C63 H63 I N7 V'
_chemical_formula_weight         1096.04
_chemical_name_common
;
Heptakis(2,6-dimethylphenyl isocyanide-\k<i>C</i>)vanadium(I) iodide'
;
_chemical_name_systematic
;
Heptakis(2,6-dimethylphenylisocyanido-\k<i>C</i>)vanadium(I)
iodide
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.765(2)
_cell_length_b                   22.765(2)
_cell_length_c                   22.101(3)
_cell_measurement_reflns_used    7505
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.023
_cell_measurement_theta_min      2.569
_cell_volume                     11454(2)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81726
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.8634
_exptl_absorpt_correction_T_min  0.6596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2003)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.550
_refine_ls_abs_structure_details
;
Flack (1983), 4655 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.002(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         10177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+6.9436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                8757
_reflns_number_total             10177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5140sup1.cif
_cod_data_source_block           I
_cod_database_code               2240550
_cod_database_fobs_code          2240550