Coordination Chemistry of 4-Methyl-2,6,7-trioxa-1-phosphabicyclo[2,2,1]heptane: Preparation and Characterization of Ru(II) Complexes
Evan E. Joslin; Claire L. McMullin; T. Brent Gunnoe; Thomas R. Cundari; Michal Sabat; William H. Myers; Inorganic Chemistry 51 (2012) 4791–4801; doi:10.1021/ic300109b

data_4328977
_publ_section_title
;
 Coordination Chemistry of
 4-Methyl-2,6,7-trioxa-1-phosphabicyclo[2,2,1]heptane: Preparation and
 Characterization of Ru(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4791
_journal_page_last               4801
_journal_paper_doi               10.1021/ic300109b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H34 B Cl3 N6 O3 P2 Ru'
_chemical_formula_weight         830.82
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.643(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5126(3)
_cell_length_b                   13.5883(3)
_cell_length_c                   17.8390(4)
_cell_measurement_reflns_used    4470
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.29
_cell_volume                     3510.77(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24938
_diffrn_reflns_theta_full        24.34
_diffrn_reflns_theta_max         24.34
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.7875
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         5709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0346
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                4461
_reflns_number_total             5709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300109b_si_004.cif
_cod_data_source_block           C32H34BN6O3P2Cl3Ru
_cod_original_cell_volume        3510.8(1)
_cod_database_code               4328977