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_7036778
_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_sum            'C43 H53 N2 Nb O2 P3'
_chemical_formula_weight         815.69
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.662(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0102(10)
_cell_length_b                   16.5289(12)
_cell_length_c                   18.0957(10)
_cell_measurement_temperature    100(2)
_cell_volume                     4186.0(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87281
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.215
_diffrn_reflns_theta_min         3.623
_diffrn_source                   'fine-focus sealed tube, graphite'
_exptl_absorpt_coefficient_mu    3.707
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.9292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6190
_reflns_number_total             7782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03383g2.cif
_cod_data_source_block           D8_10142_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036776--7036781.cif.'
_cod_database_code               7036778
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.708
_shelxl_version_number           2014-2
_shelx_res_checksum              3207