Stable Carbene and Diazoalkane Complexes of the Same Complex System. Synthesis, Structure, and Reactivity of PNP−Ru(II) Fluorenylidene and Diazofluorene Complexes
Zhang, Jing; Gandelman, Mark; Shimon, Linda J. W.; Milstein, David; Organometallics 27 (2008) 3526–; doi:10.1021/om800294v

data_4071653
_publ_section_title
;
 Stable Carbene and Diazoalkane Complexes of the Same Complex System.
 Synthesis, Structure, and Reactivity of PNP&#x2212;Ru(II) Fluorenylidene
 and Diazofluorene Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3526
_journal_paper_doi               10.1021/om800294v
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C36 H51 Cl N P2 Ru, C H2 Cl2, B F4'
_chemical_formula_sum            'C37 H53 B Cl3 F4 N P2 Ru'
_chemical_formula_weight         867.97
_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                 109.116(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.659(1)
_cell_length_b                   15.011(1)
_cell_length_c                   16.4730(9)
_cell_measurement_reflns_used    16507
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.77
_cell_measurement_theta_min      2.55
_cell_volume                     3892.2(4)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (BrukerNonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean HKL
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       HKL
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16507
_diffrn_reflns_theta_full        20.77
_diffrn_reflns_theta_max         20.77
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0000P)^2^+17.6733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3313
_reflns_number_total             3955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800294v-file001.cif
_cod_data_source_block           m347
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4071653