Synthesis and Reactivity of Phosphinocarbyne Complexes
Colebatch, Annie L.; Hill, Anthony F.; Sharma, Manab; Organometallics 34 (2015) 2165–; doi:10.1021/om500833n

data_4084450
_publ_section_title
;
 Synthesis and Reactivity of Phosphinocarbyne Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2165
_journal_paper_doi               10.1021/om500833n
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C31 H36 B2 Cl3 N6 O2 P1 W1'
_chemical_formula_sum            'C31 H36 B2 Cl3 N6 O2 P W'
_chemical_formula_weight         867.47
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
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_cell_angle_beta                 92.6882(10)
_cell_angle_gamma                105.8832(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2173(2)
_cell_length_b                   10.4412(2)
_cell_length_c                   17.5622(3)
_cell_measurement_reflns_used    41945
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     1799.87(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49059
_diffrn_reflns_theta_full        30.039
_diffrn_reflns_theta_max         30.039
_diffrn_reflns_theta_min         2.700
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.44
_refine_diff_density_min         -2.92
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9939
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         10525
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.0017820
_refine_ls_shift/su_mean         0.0000688
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.78P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0894
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0894
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8636
_reflns_number_total             10526
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.22
_oxford_diffrn_Wilson_scale      36.21
_oxford_refine_ls_r_factor_ref   0.0582
_oxford_refine_ls_scale          0.20343(8)
_oxford_reflns_number_all        10525
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om500833n_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/COD-crude-data--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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084449--4084453.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C31 H36 B2 Cl3 N6 O2 P1 W1'
_cod_database_code               4084450
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;