Synthesis of a Cobalt−Phospholyl Half-Sandwich Complex and Its Transformation into a Phosphacobaltocene
Cabon, Yves; Carmichael, Duncan; Forissier, Kareen; Mathey, François; Ricard, Louis; Seeboth, Nicolas; Organometallics 26 (2007) 5468–; doi:10.1021/om0610952

data_4072856
_publ_section_title
;
 Synthesis of a Cobalt&#x2212;Phospholyl Half-Sandwich Complex and Its
 Transformation into a Phosphacobaltocene
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5468
_journal_paper_doi               10.1021/om0610952
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C17 H27 Co O2 P'
_chemical_formula_weight         353.29
_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                68.120(5)
_cell_angle_beta                 85.680(5)
_cell_angle_gamma                79.930(5)
_cell_formula_units_Z            2
_cell_length_a                   9.380(5)
_cell_length_b                   10.174(5)
_cell_length_c                   10.251(5)
_cell_measurement_reflns_used    157
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     893.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full .984
_diffrn_measured_fraction_theta_max .984
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6764
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.8333
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.348
_refine_diff_density_min         -.396
_refine_diff_density_rms         .067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         5125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0367P)^2^+0.5137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                4363
_reflns_number_total             5125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0610952-file001.cif
_cod_data_source_block           copac
_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_sg_symbol_H-M      'P-1      '
_cod_database_code               4072856