Towards inert and preorganized d-block-containing receptors for trivalent lanthanides: The synthesis and characterization of triple-helical monometallic OsII and bimetallic OsII–LnIII complexes
Riis-Johannessen, Thomas; Dupont, Nathalie; Canard, Gabriel; Bernardinelli, Gérald; Hauser, Andreas; Piguet, Claude; Dalton Transactions  (2008) 3661–3677; doi:10.1039/b718885d

data_7003707
_publ_section_title
;
 Towards inert and preorganized d-block-containing receptors for
 trivalent lanthanides: The synthesis and characterization of
 triple-helical monometallic OsII and bimetallic OsII--LnIII complexes
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              3661
_journal_page_last               3677
_journal_paper_doi               10.1039/b718885d
_journal_year                    2008
_chemical_formula_moiety
;
(C42 H39 N9 Os), (F6 P)2
;
_chemical_formula_sum            'C42 H39 F12 N9 Os P2'
_chemical_formula_weight         1149.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.243(9)
_cell_length_b                   10.705(2)
_cell_length_c                   20.753(4)
_cell_measurement_reflns_used    5672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.257
_cell_measurement_theta_min      4.415
_cell_volume                     8541(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'frames each covering 0.3\% in\w'
_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  0.0915
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46976
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    3.159
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.852487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.751
_refine_diff_density_min         -2.174
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                7090
_reflns_number_total             9795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718885d.txt
_cod_data_source_block           cr28007m
_cod_original_cell_volume        8541(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7003707