Aminoallenylidene complexes of ruthenium(II) from the regioselective addition of secondary amines to butatrienylidene intermediates: a combined experimental and theoretical study of the hindered rotation around the CN-bond
Rainer F. Winter; Stephan Hartmann; Stanislav Záliš; Karl Wilhelm Klinkhammer; Dalton Trans.  (2003) 2342–2352; doi:10.1039/b211774f

data_7012531
_publ_section_title
;
 Aminoallenylidene complexes of ruthenium(II) from the regioselective
 addition of secondary amines to butatrienylidene intermediates: a
 combined experimental and theoretical study of the hindered rotation
 around the CN-bond
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2342
_journal_page_last               2352
_journal_paper_doi               10.1039/b211774f
_journal_year                    2003
_chemical_formula_sum            'C62 H57 Cl F6 N P4 Ru Sb'
_chemical_formula_weight         1312.24
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.557(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8677(9)
_cell_length_b                   24.811(3)
_cell_length_c                   21.3714(16)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     6540.1(10)
_computing_cell_refinement       'Siemens XScans'
_computing_data_collection       'Siemens XScans'
_computing_data_reduction        'Siemens XScans'
_computing_molecular_graphics    'Bruker Shelxtl 5.1 - XP'
_computing_publication_material  'Bruker Shelxtl'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens P4 4-circle-diffractometer'
_diffrn_measurement_method       '\w 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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12324
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.835
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         10209
_refine_ls_number_restraints     979
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                6170
_reflns_number_total             10209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211774f.txt
_cod_data_source_block           diffoq
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6540.3(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012531