Structural Characterization of (C5H5)Co(PPh3)(η2-alkyne) and (C5H5)Co(η2-alkyne) Complexes of Highly Polarized Alkynes
Baldridge, Kim K.; Bunker, Kevin D.; Vélez, Carmen L.; Holland, Ryan L.; Rheingold, Arnold L.; Moore, Curtis E.; O’Connor, Joseph M.; Organometallics 32 (2013) 5473–; doi:10.1021/om400749g

data_4081653
_publ_section_title
;
 Structural Characterization of (C5H5)Co(PPh3)(\h2-alkyne) and
 (C5H5)Co(\h2-alkyne) Complexes of Highly Polarized Alkynes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5473
_journal_paper_doi               10.1021/om400749g
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C34 H34 Co O2 P S Si'
_chemical_formula_sum            'C34 H34 Co O2 P S Si'
_chemical_formula_weight         624.66
_chemical_name_systematic
; 
  Olex2 1.2-beta 
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466) 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_date             2013-07-15
_audit_creation_method
; 
  Olex2 1.2-beta 
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466) 
;
_cell_angle_alpha                90
_cell_angle_beta                 95.579(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5612(12)
_cell_length_b                   17.853(2)
_cell_length_c                   16.0829(19)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.550
_cell_measurement_theta_min      2.281
_cell_volume                     3018.1(6)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics
; 
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, 
OLEX2: a complete structure solution, refinement and analysis program. 
J. Appl. Cryst. (2009). 42, 339-341. 
;
_computing_publication_material
; 
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, 
OLEX2: a complete structure solution, refinement and analysis program. 
J. Appl. Cryst. (2009). 42, 339-341. 
;
_computing_structure_refinement
; 
XL, G.M. Sheldrick, Acta Cryst. 
(2008). A64, 112-122 
;
_computing_structure_solution
; 
XS, G.M. Sheldrick, Acta Cryst. 
(2008). A64, 112-122 
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26319
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.550
_diffrn_reflns_theta_min         1.709
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0619 before and 0.0562 after correction. 
The Ratio of minimum to maximum transmission is 0.9147. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            Brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+1.9743P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4458
_reflns_number_total             5625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400749g_si_001.cif
_cod_data_source_block           RLH3004
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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_crystal_colour_primary' value 'Brown' changed to
'brown' 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 
;
_cod_original_cell_volume        3018.0(6)
_cod_database_code               4081653
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Aromatic/amide H refined with riding coordinates: 
 C13(H13), C32(H32), C18(H18), C11(H11), C7(H7), C26(H26), C27(H27), C34(H34), 
 C9(H9), C16(H16), C8(H8), C19(H19), C33(H33), C28(H28), C14(H14), C20(H20), 
 C25(H25), C24(H24), C31(H31), C30(H30), C10(H10), C15(H15), C12(H12), C22(H22), 
  C21(H21) 
2.b Idealised Me refined as rotating group: 
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C) 
;
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.896
_shelx_hkl_checksum              73512
_shelx_res_checksum              84258
_shelxl_version_number           2013-2