Bis(pyrene)metal complexes of vanadium, niobium and titanium: isolable homoleptic pyrene complexes of transition metals
Kucera, Benjamin E.; Jilek, Robert E.; Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614015290

data_2019611
_publ_section_title
;
 Bis(pyrene)metal complexes of vanadium, niobium and titanium: isolable
 homoleptic pyrene complexes of transition metals
;
_journal_coeditor_code           WQ3068
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614015290
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Nb (C16 H10)2]'
_chemical_formula_moiety         'C32 H20 Nb'
_chemical_formula_sum            'C32 H20 Nb'
_chemical_formula_weight         497.39
_chemical_name_common            7057
_chemical_name_systematic
;
Bis[(1,2,3,3a,10a,10b-\h)-pyrene]niobium(0)
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 105.554(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5838(12)
_cell_length_b                   9.5974(13)
_cell_length_c                   12.8876(18)
_cell_measurement_reflns_used    2133
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.46
_cell_volume                     1022.8(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)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9829
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.055
_diffrn_reflns_theta_min         2.463
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.8386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       needle
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0302P)^2^+1.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                1360
_reflns_number_total             1814
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3068sup1.cif
_cod_data_source_block           II
_cod_database_code               2019611
_cod_database_fobs_code          2019611
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              94402
_shelx_res_checksum              92886
_shelxl_version_number           2.014