Oxo-Bridged Bis(group 4 metal unsymmetric phosphonium-stabilized carbene) Complexes
Guo, Jia-Yi; Chan, Yuk-Chi; Li, Yongxin; Ganguly, Rakesh; So, Cheuk-Wai; Organometallics 34 (2015) 1238–; doi:10.1021/om5012962

data_4085619
_publ_section_title
;
 Oxo-Bridged Bis(group 4 metal unsymmetric phosphonium-stabilized carbene)
 Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1238
_journal_paper_doi               10.1021/om5012962
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C60 H70 N4 O P4 S2 Si2 Zr2,0.7(C4 H10 O),0.3(C7 H8)'
_chemical_formula_sum            'C64.9 H79.4 N4 O1.7 P4 S2 Si2 Zr2'
_chemical_formula_weight         1369.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 92.501(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6988(5)
_cell_length_b                   17.7746(7)
_cell_length_c                   14.4923(6)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      37.06
_cell_measurement_theta_min      2.46
_cell_volume                     3268.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69745
_diffrn_reflns_theta_full        37.08
_diffrn_reflns_theta_max         37.08
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.8063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1421
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.255
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.032(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         30455
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                27441
_reflns_number_total             30455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5012962_si_002.cif
_cod_data_source_block           scw259s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 4085616--4085622.cif.
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C64.90 H79.40 N4 O1.70 P4 S2 Si2 Zr2'
_cod_database_code               4085619