Assembly and stabilization of {E(cyclo-P3)2} (E = Sn, Pb) as a bridging ligand spanning two triaryloxyniobium units.
Velian, Alexandra; Cossairt, Brandi M.; Cummins, Christopher C.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1891–1895; doi:10.1039/c5dt03383g

data_7036776
_publ_section_title
;
 Assembly and stabilization of {E(cyclo-P3)2} (E = Sn, Pb) as a bridging
 ligand spanning two triaryloxyniobium units.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1891
_journal_page_last               1895
_journal_paper_doi               10.1039/c5dt03383g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C82 H112 N2 Nb2 O6 P6, (C6 H6)'
_chemical_formula_sum            'C88 H118 N2 Nb2 O6 P6'
_chemical_formula_weight         1749.6787
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-30 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                94.9290(10)
_cell_angle_beta                 93.6830(10)
_cell_angle_gamma                95.8840(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4029(7)
_cell_length_b                   13.7294(10)
_cell_length_c                   16.3434(12)
_cell_measurement_temperature    100(2)
_cell_volume                     2307.1(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         11436
_refine_ls_number_restraints     986
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0234P)^2^+1.5512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8015
_reflns_number_total             11436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03383g2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7036776--7036781.cif.'
_cod_database_code               7036776
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.984
_exptl_absorpt_special_details   ;
_shelx_res_checksum              73044