Synthesis and Structural Characterization of Group 4 Metal Complexes Bearing Pentavalent Phosphorus-Bridged Ligands [(C13H8)(iPr2N)P(−O)(C2B10H10)]2−and [(C13H9)(iPr2N)P(O)(C2B9H10)]2−
Wang, Hong; Shen, Hao; Chan, Hoi-Shan; Xie, Zuowei; Organometallics 27 (2008) 3964–; doi:10.1021/om800319w

data_4071695
_publ_section_title
;
 Synthesis and Structural Characterization of Group 4 Metal Complexes
 Bearing Pentavalent Phosphorus-Bridged Ligands
 [(C13H8)(iPr2N)P(&#x2212;O)(C2B10H10)]2&#x2212;and
 [(C13H9)(iPr2N)P(&#xE5FB;O)(C2B9H10)]2&#x2212;
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3964
_journal_paper_doi               10.1021/om800319w
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C33 H60 B10 N3 O3 P Zr'
_chemical_formula_weight         777.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.732(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0355(6)
_cell_length_b                   26.3259(17)
_cell_length_c                   17.6070(11)
_cell_measurement_temperature    293(2)
_cell_volume                     4167.2(5)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.1179
_diffrn_reflns_av_sigmaI/netI    0.1300
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20528
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.606041
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1899
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+14.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.3111
_reflns_number_gt                3077
_reflns_number_total             6539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800319w-file001.cif
_cod_data_source_block           5(THF)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4071695