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_4328976
_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            'C18 H29 Cl6 O3 P Ru'
_chemical_formula_weight         638.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.3120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7611(3)
_cell_length_b                   10.4473(3)
_cell_length_c                   22.4999(6)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      35.94
_cell_measurement_theta_min      2.68
_cell_volume                     2496.20(12)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            27747
_diffrn_reflns_theta_full        36.16
_diffrn_reflns_theta_max         36.16
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.8332
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       platel
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         7924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.000
_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          0.0965
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                7317
_reflns_number_total             11527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300109b_si_003.cif
_cod_data_source_block           C18H29Cl6O3PRu
_cod_database_code               4328976