Insertion of Isocyanate and Isothiocyanate into the Ln‒P σ-Bond of Organolanthanide Phosphides
Yi, Weiyin; Zhang, Jie; Hong, Longcheng; Chen, Zhenxia; Zhou, Xigeng; Organometallics 30 (2011) 5809–; doi:10.1021/om2006722

data_4065274
_publ_section_title
;
 Insertion of Isocyanate and Isothiocyanate into the Ln--P \s-Bond of
 Organolanthanide Phosphides
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5809
_journal_paper_doi               10.1021/om2006722
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C46 H50 B N7 P S Y'
_chemical_formula_weight         863.68
_chemical_name_systematic
; 
 ? 
;
_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                76.376(5)
_cell_angle_beta                 82.472(5)
_cell_angle_gamma                66.392(5)
_cell_formula_units_Z            2
_cell_length_a                   11.212(4)
_cell_length_b                   13.638(5)
_cell_length_c                   16.428(6)
_cell_measurement_reflns_used    798
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.479
_cell_measurement_theta_min      2.553
_cell_volume                     2235.1(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.1288
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10116
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_T_max  0.9193
_exptl_absorpt_correction_T_min  0.8144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8515
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                4166
_reflns_number_total             8515
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4065273
_cod_data_source_file            om2006722_si_001.cif
_cod_data_source_block           a10405a
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2235.1(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065274