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_4081652
_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         'C41 H48 Co O2 P S Si'
_chemical_formula_sum            'C41 H48 Co O2 P S Si'
_chemical_formula_weight         722.84
_chemical_name_systematic
; 
  Olex2 1.2-beta 
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466) 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2013-07-15
_audit_creation_method
; 
  Olex2 1.2-beta 
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466) 
;
_cell_angle_alpha                93.231(2)
_cell_angle_beta                 92.647(2)
_cell_angle_gamma                92.913(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5763(16)
_cell_length_b                   10.6836(16)
_cell_length_c                   16.640(3)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.32
_cell_volume                     1872.5(5)
_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 0.980
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device       'Siemens P4 Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0429
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14397
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.132
_diffrn_reflns_theta_min         1.912
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.6732P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7233
_reflns_number_total             8314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400749g_si_001.cif
_cod_data_source_block           CLV276_34
_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 'Orange' changed
to 'orange' 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_database_code               4081652
_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 Ternary CH refined with riding coordinates: 
 C10(H10), C11(H11), C12(H12) 
2.b Aromatic/amide H refined with riding coordinates: 
 C4(H4), C5(H5), C7(H7), C8(H8), C19(H19), C23(H23), C22(H22), C21(H21), 
 C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), 
  C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41) 
2.c Idealised Me refined as rotating group: 
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B, 
 H16C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C) 
;
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.879
_shelx_hkl_checksum              28213
_shelx_res_checksum              52063
_shelxl_version_number           2013-2