Ruthenium Trispyrazolylborate Complexes. 18.1Aminocarbene Ruthenium Complexes Derived from Terminal Alkynes and 2-Aminopyridines
Rüba, Eva; Hummel, Alexandra; Mereiter, Kurt; Schmid, Roland; Kirchner, Karl; Organometallics 21 (2002) 4955–; doi:10.1021/om020441m

data_4077030
_publ_section_title
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 Ruthenium Trispyrazolylborate Complexes. 18.1Aminocarbene Ruthenium
 Complexes Derived from Terminal Alkynes and 2-Aminopyridines
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_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              4955
_journal_paper_doi               10.1021/om020441m
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C30 H36 B2 Cl2 N16 Ru2, 2(C4 H10 O)'
_chemical_formula_sum            'C38 H56 B2 Cl2 N16 O2 Ru2'
_chemical_formula_weight         1063.64
_chemical_name_common
'[RuTp(m-apic)Cl]2.2(O(C2H5)2)  =   (5b.2(O(C2H5)2)'
_chemical_name_systematic
; 
 ?
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_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.674(4)
_cell_length_b                   16.711(4)
_cell_length_c                   17.955(4)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.6
_cell_volume                     4703(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, and XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'BRUKER SMART 3-circle with 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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            73636
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   'semi-empirical from equivalents (SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00003(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6701
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+8.2506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                4586
_reflns_number_total             6701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020441m.cif
_cod_data_source_block           5b
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
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_cod_original_cell_volume        4702.9(19)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077030