1,1,2,2,2,3,3,3-Octacarbonyl-1,1,2,3-tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.1^3,7^]decane-κ<i>P</i>)-<i>triangulo</i>-triosmium(0)
Marolf, David M.; Brehm, Kristen L.; Lynch, Vincent M.; Powell, Gregory L.; IUCrData 5 (2020) x200935–; doi:10.1107/S2414314620009359

data_1558619
_publ_section_title
;
 1,1,2,2,2,3,3,3-Octacarbonyl-1,1,2,3-tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.1^3,7^]decane-\k<i>P</i>)-<i>triangulo</i>-triosmium(0)
;
_journal_coeditor_code           WM4135
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x200935
_journal_paper_doi               10.1107/S2414314620009359
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '[Os3 (C6 H12 N3 P)4 (C O)8]'
_chemical_formula_moiety         'C32 H48 N12 O8 Os3 P4 '
_chemical_formula_sum            'C32 H48 N12 O8 Os3 P4'
_chemical_formula_weight         1423.30
_chemical_name_common            Os3(CO)8(PTA)4
_chemical_name_systematic
1,1,2,2,2,3,3,3-Octacarbonyl-1,1,2,3-tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.1^3,7^]decane-\k<i>P</i>)-<i>triangulo</i>-triosmium(0)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7500(2)
_cell_length_b                   15.8889(2)
_cell_length_c                   27.5984(3)
_cell_measurement_reflns_used    21014
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1
_cell_measurement_theta_min      3.94
_cell_volume                     8222.03(16)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2016)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2016)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2016)
;
_computing_molecular_graphics
;
XP in <i>SHELXTL/PC</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick 2015)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick 2015)
;
_computing_structure_solution
;
<i>SUPERFLIP</i> (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38755
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.273
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    19.162
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2016)
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    2.300
_exptl_crystal_description       plates
_exptl_crystal_F_000             5408
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.239
_refine_diff_density_min         -1.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+60.4468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                7535
_reflns_number_total             8184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4135sup1.cif
_cod_data_source_block           I
_cod_database_code               1558619
_shelx_hkl_checksum              3937
_shelx_res_checksum              52665
_cod_database_fobs_code 1558619