Osmium(II) Complexes Containing a Dianionic CCCC-Donor Tetradentate Ligand
Alabau, Roberto G.; Esteruelas, Miguel A.; Oliván, Montserrat; Oñate, Enrique; Palacios, Adrián U.; Tsai, Jui-Yi; Xia, Chuanjun; Organometallics 35 (2016) 3981–; doi:10.1021/acs.organomet.6b00776

data_4089167
_publ_section_title
;
 Osmium(II) Complexes Containing a Dianionic CCCC-Donor Tetradentate
 Ligand
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              3981
_journal_paper_doi               10.1021/acs.organomet.6b00776
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety
'4(C48 H41 N4 Os P2), 4(C F3 O3 S), C2 H4 Cl4, 2(C2 H3 N)'
_chemical_formula_sum            'C50.5 H43.5 Cl F3 N4.5 O3 Os P2 S'
_chemical_formula_weight         1138.05
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/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                 108.6970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5713(14)
_cell_length_b                   19.295(2)
_cell_length_c                   18.4609(19)
_cell_measurement_reflns_used    7943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4579.0(8)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55736
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.020
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         11059
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+10.0232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                8625
_reflns_number_total             11059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00776_si_002.cif
_cod_data_source_block           11-enrique211
_cod_original_cell_volume        4579.1(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C50.50 H43.50 Cl F3 N4.50 O3 Os P2 S'
_cod_database_code               4089167