Phosphaalkenes as Long-Lived Phosphorus Cluster Surface Functional Groups: Intramolecular P=C Addition to a Niobium-Supported P7 Cage
Brandi M. Cossairt; Christopher C. Cummins; Inorganic Chemistry 47 (2008) 9363–9371; doi:10.1021/ic8009282

data_4305987
_publ_contact_author_address
;Department of Chemistry 
Building 6-435
77 Massachusetts Avenue
Cambridge, MA 02139, USA
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_fax         617-253-7670
_publ_contact_author_name        'Professor Christopher C. Cummins'
_publ_contact_author_phone       617-253-5332
_publ_section_title
;
Phosphaalkenes as Long-Lived Phosphorus Cluster Surface Functional Groups:
Intramolecular P=C Addition to a Niobium-Supported P7 Cage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9363
_journal_page_last               9371
_journal_paper_doi               10.1021/ic8009282
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C67 H92.5 Nb O5.75'
_chemical_formula_weight         1082.82
_chemical_name_common            ONb(OC[Ad]Mes)3(OEt2)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                73.720(4)
_cell_angle_beta                 78.872(4)
_cell_angle_gamma                80.224(4)
_cell_formula_units_Z            2
_cell_length_a                   12.592(3)
_cell_length_b                   14.536(3)
_cell_length_c                   17.436(4)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2983.1(12)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.1004
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41641
_diffrn_reflns_theta_full        23.36
_diffrn_reflns_theta_max         23.36
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1163
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     875
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1073P)^2^+1.6330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1830
_reflns_number_gt                6186
_reflns_number_total             8618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8009282_si_001_1.cif
_cod_data_source_block           07016
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C67 H92.50 Nb O5.75'
_cod_database_code               4305987