Reductive Labilization of a Cyclometalating Ligand Applied to Auxiliary-Mediated Asymmetric Coordination Chemistry
Kraack, Marianne; Harms, Klaus; Meggers, Eric; Organometallics 32 (2013) 5103–; doi:10.1021/om4006627

data_4081390
_publ_section_title
;
 Reductive Labilization of a Cyclometalating Ligand Applied to
 Auxiliary-Mediated Asymmetric Coordination Chemistry
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5103
_journal_paper_doi               10.1021/om4006627
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_sum            'C68 H67 B N6 O4 Ru'
_chemical_formula_weight         1144.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6846(14)
_cell_length_b                   14.8157(18)
_cell_length_c                   28.691(4)
_cell_measurement_reflns_used    6365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.47
_cell_measurement_theta_min      1.42
_cell_volume                     5817.0(12)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3062
_diffrn_reflns_av_unetI/netI     0.5071
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.419
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  1.1356
_exptl_absorpt_correction_T_min  0.8875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] 
;
_exptl_crystal_colour            red
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_exptl_crystal_description       needle
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_refine_diff_density_max         0.724
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.587
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         10543
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      0.576
_refine_ls_R_factor_all          0.2344
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1418
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_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2506
_reflns_number_total             10543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4006627_si_001.cif
_cod_data_source_block           L-{S}-7
_cod_original_cell_volume        5817.0(13)
_cod_database_code               4081390
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2012-9
_shelx_res_checksum              25034
_shelx_hkl_checksum              85194