Hydrogen Atom Transfer Reactions of the Unsaturated Hydroxycarbyne Complex [W2Cp2(μ-COH)(μ-PPh2)2]BF4
Cimadevilla, Fernanda; García, M. Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Graiff, Claudia; Tiripicchio, Antonio; Organometallics 32 (2013) 4624–; doi:10.1021/om400598m

data_4081332
_publ_section_title
;
 Hydrogen Atom Transfer Reactions of the Unsaturated Hydroxycarbyne
 Complex [W2Cp2(\m-COH)(\m-PPh2)2]BF4
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4624
_journal_paper_doi               10.1021/om400598m
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C42 H38 B F4 N O P2 W2'
_chemical_formula_weight         1089.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.29(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.662(3)
_cell_length_b                   20.723(5)
_cell_length_c                   17.943(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      6
_cell_volume                     3940.6(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Siemens AED'
_diffrn_measurement_method       'teta 2 teta 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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7055
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        'no decay observed'
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    5.968
_exptl_absorpt_correction_T_max  0.3411
_exptl_absorpt_correction_T_min  0.1623
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                4649
_reflns_number_total             6839
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400598m_si_002.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4081332
_exptl_absorpt_factor_mur        1.492
_exptl_absorpt_correction_t_ave  0.2357
_exptl_absorpt_rmerge_before     0.1120
_exptl_absorpt_rmerge_after      0.0884