Preparation of Phosphorescent Osmium(IV) Complexes with N,N′,C- and C,N,C′-Pincer Ligands
Alabau, Roberto G.; Esteruelas, Miguel A.; Oliván, Montserrat; Oñate, Enrique; Organometallics 36 (2017) 1848–; doi:10.1021/acs.organomet.7b00193

data_4089298
_publ_section_title
;
 Preparation of Phosphorescent Osmium(IV) Complexes with N,N&#x2032;,C-
 and C,N,C&#x2032;-Pincer Ligands
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1848
_journal_paper_doi               10.1021/acs.organomet.7b00193
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C32 H53 N3 Os P2, 2(C H4 O)'
_chemical_formula_sum            'C34 H61 N3 O2 Os P2'
_chemical_formula_weight         795.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 98.2780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9732(8)
_cell_length_b                   13.4054(6)
_cell_length_c                   16.3797(8)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3688.1(3)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.936
_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  0.0408
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42643
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.726
_diffrn_reflns_theta_min         2.218
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.718
_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            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.916
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8943
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+3.5189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7625
_reflns_number_total             8943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00193_si_002.cif
_cod_data_source_block           complex_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089298
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.518
_shelx_estimated_absorpt_t_max   0.657
_shelx_res_checksum              65983
_shelx_hkl_checksum              57962