Synthesis and characterisation of group 8 tris(1-benzyl-1,2,3-triazol-4-yl)-p-anisoylmethane complexes
Francis, Samuel; Rice, Craig; Scattergood, Paul A.; Elliott, Paul; Dalton Transactions  (2022) –; doi:10.1039/D2DT02503E

data_7711039
_publ_section_title
;
 Synthesis and characterisation of group 8
 tris(1-benzyl-1,2,3-triazol-4-yl)-p-anisoylmethane complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02503E
_journal_year                    2022
_chemical_formula_sum            'C78 H68 F12 N22 O2 Os P2'
_chemical_formula_weight         1825.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-07 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                95.897(10)
_cell_angle_beta                 94.850(9)
_cell_angle_gamma                92.366(14)
_cell_formula_units_Z            1
_cell_length_a                   11.866(3)
_cell_length_b                   12.902(3)
_cell_length_c                   12.921(3)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.25
_cell_volume                     1958.1(8)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.595
_diffrn_reflns_theta_min         2.125
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.484
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.9582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11329
_reflns_number_total             11883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02503e2.cif
_cod_data_source_block           mo_PIPE_Os_tripod_0m_a
_cod_original_cell_volume        1958.2(9)
_cod_database_code               7711039
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              89015