Formation of P–H, P–C, and C–H Bonds by Hydride Attack on a Electrophilic Phosphide-Bridged Dimolybdenum Complex. Trapping the Phosphinidene Ligand with Borane
Amor, Inmaculada; García-Vivó, Daniel; García, M. Esther; Ruiz, Miguel A.; Sáez, David; Hamidov, Hayrullo; Jeffery, John C.; Organometallics 26 (2007) 466–468; doi:10.1021/om061097m

data_4082253
_publ_section_title
;
 Formation of P--H, P--C, and C--H Bonds by Hydride Attack on a
 Electrophilic Phosphide-Bridged Dimolybdenum Complex.
 Trapping the Phosphinidene Ligand with Borane
;
_journal_coden_ASTM              ORGND7
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              466
_journal_page_last               468
_journal_paper_doi               10.1021/om061097m
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C30 H44 B Mo2 O2 P'
_chemical_formula_sum            'C30 H44 B Mo2 O2 P'
_chemical_formula_weight         670.31
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.3514(5)
_cell_length_b                   17.7124(8)
_cell_length_c                   29.7652(14)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.10
_cell_measurement_theta_min      2.90
_cell_volume                     5984.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.602
_diffrn_detector_type            'Bruker-AXS SMART 6000'
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      'frames, 0.3\% width'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS D8'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass fibre'
_diffrn_radiation_collimation    'Osmic CMF12-38Cu6 (blue) mirror optics'
_diffrn_radiation_monochromator  'Osmic CMF12-38Cu6 (blue) mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24009
_diffrn_reflns_theta_full        70.19
_diffrn_reflns_theta_max         70.19
_diffrn_reflns_theta_min         2.90
_diffrn_source                   rotating-anode
_diffrn_source_current           120
_diffrn_source_power             4.8
_diffrn_source_size              '3 x 0.3mm'
_diffrn_source_target            Cu
_diffrn_source_type              'MAC Science M18XCE'
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    7.547
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                9028
_reflns_number_total             9836
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4072858
_cod_data_source_file            om061097msup1.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_diffrn_radiation_probe' value 'X-ray' changed to
'x-ray' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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 

The following automatic conversions were performed:

data name '_diffrn_specimen_support' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4082253