Easy Access to Bio-Inspired Osmium(II) Complexes through Electrophilic Intramolecular C(sp2)-H Bond Cyclometalation
Ricardo Cerón-Camacho; David Morales-Morales; Simon Hernández; Ronan Le Lagadec; Alexander D. Ryabov; Inorganic Chemistry 47 (2008) 4988–4995; doi:10.1021/ic800251t

data_4305053
_publ_contact_author_address
;     Instituto de Qu\'imica
      Universidad Nacional Aut\'onoma de M\'exico
      Circuito Exterior, CU
      M\'exico, D.F. 04510
      M\'exico
;
_publ_contact_author_email       simonho@servidor.unam.mx
_publ_contact_author_fax         '+(5255) 56162215'
_publ_contact_author_name        'Hern\'andez-Ortega, Simon'
_publ_contact_author_phone       '+(5255) 56162203'
_publ_section_title
;
Easy Access to Bio-Inspired Osmium(II) Complexes through Electrophilic
Intramolecular C(sp2)-H Bond Cyclometalation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4988
_journal_page_last               4995
_journal_paper_doi               10.1021/ic800251t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C25 H26 N5 Os, F6 P'
_chemical_formula_sum            'C25 H26 F6 N5 Os P'
_chemical_formula_weight         731.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 96.271(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2693(7)
_cell_length_b                   12.4643(8)
_cell_length_c                   18.8585(12)
_cell_measurement_reflns_used    6453
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      30.88
_cell_measurement_theta_min      2.44
_cell_volume                     2633.1(3)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_publication_material  'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_structure_refinement  'SHELXTL V 6.14 (Sheldrick, 2006)'
_computing_structure_solution    'SHELXTL V 6.14 (Sheldrick, 2006)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 0.65
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  0.7327
_exptl_absorpt_correction_T_min  0.4402
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SHELXTL V 6.14 (Sheldrick, 2006)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.033(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                3622
_reflns_number_total             4597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800251t-file002_3.cif
_cod_data_source_block           COMPOUND_6B
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Analytical' changed
to 'analytical' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'No' 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 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4305053
_solved_by                       'Simon Hernandez-Ortega'