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_2019612
_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          '[K Ti (C16 H10)2 (C12 H24 O6)]'
_chemical_formula_moiety         'C12 H24 K O6 +, C32 H20 Ti -'
_chemical_formula_sum            'C44 H44 K O6 Ti'
_chemical_formula_weight         755.79
_chemical_name_common            7226
_chemical_name_systematic
<i>catena</i>-Poly[[(18-crown-6)potassium]-\m-[(1,2-\h:1,2,3,3a,10a,10b-\h)-pyrene]-titanate(I)-\m-[(1,2,3,3a,10a,10b-\h:6,7-\h)-pyrene]]
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 111.084(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3934(13)
_cell_length_b                   15.682(2)
_cell_length_c                   11.3559(14)
_cell_measurement_reflns_used    2393
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.23
_cell_volume                     1727.0(4)
_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    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0457
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19900
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2012)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0529P)^2^+0.8538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2929
_reflns_number_total             3941
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3068sup1.cif
_cod_data_source_block           III
_cod_database_code               2019612
_cod_database_fobs_code          2019612
_shelx_estimated_absorpt_t_min   0.884
_shelx_estimated_absorpt_t_max   0.920
_shelx_hkl_checksum              10278
_shelx_res_checksum              67971
_shelxl_version_number           2.014