Preparation of Diazoalkane Complexes of Ruthenium and Their Cyclization Reactions with Alkenes and Alkynes
Albertin, Gabriele; Antoniutti, Stefano; Botter, Alessandra; Castro, Jesús; Giacomello, Mattia; Organometallics  (2014) 140702103357007–; doi:10.1021/om500481d

data_4083867
_publ_section_title
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 Preparation of Diazoalkane Complexes of Ruthenium and Their
 Cyclization Reactions with Alkenes and Alkynes
;
_journal_name_full               Organometallics
_journal_page_first              140702103357007
_journal_paper_doi               10.1021/om500481d
_journal_year                    2014
_chemical_formula_sum            'C67 H64 B N3 O3 P2 Ru'
_chemical_formula_weight         1133.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                87.2064(15)
_cell_angle_beta                 79.1701(11)
_cell_angle_gamma                75.3412(12)
_cell_formula_units_Z            2
_cell_length_a                   13.2351(5)
_cell_length_b                   13.9082(5)
_cell_length_c                   16.4809(6)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      68.01
_cell_measurement_theta_min      2.73
_cell_volume                     2882.72(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80446
_diffrn_reflns_theta_full        68.26
_diffrn_reflns_theta_max         68.26
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.108
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         10159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0577P)^2^+0.8014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                9599
_reflns_number_total             10159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500481d_si_002.cif
_cod_data_source_block           19b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Triclinic'' was replaced with
'triclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083867