Mono- and Dimetalation of a Tridentate Bisimidazole-Phosphine Ligand
Flowers, Sarah E.; Cossairt, Brandi M.; Organometallics 33 (2014) 4341–; doi:10.1021/om500592u

data_4084289
_publ_section_title
;
 Mono- and Dimetalation of a Tridentate Bisimidazole-Phosphine Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4341
_journal_paper_doi               10.1021/om500592u
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C38 H46 N4 P Ru, 0.31(C4 H10 O), 0.69(C4 H8 O), Cl'
_chemical_formula_sum            'C42 H54.63 Cl N4 O P Ru'
_chemical_formula_weight         799.02
_chemical_name_common            sef1_99a
_chemical_name_systematic
;
 sef1_99a
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-11-14T11:47:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.634(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1738(18)
_cell_length_b                   13.9542(15)
_cell_length_c                   17.0592(18)
_cell_measurement_reflns_used    1205
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3846.1(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.1646
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16464
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         26.7
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.9464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1675.5
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         15795
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+5.8237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                10398
_reflns_number_total             15795
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500592u_si_001.cif
_cod_data_source_block           twin4
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4084289