Half-sandwich complexes of osmium containing guanidine-derived ligands.
Parker, Amie; Lamata, Pilar; Viguri, Fernando; Rodríguez, Ricardo; López, José A; Lahoz, Fernando J.; García-Orduña, Pilar; Carmona, Daniel; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13601–13617; doi:10.1039/d0dt02713h

data_7705482
_publ_section_title
;
 Half-sandwich complexes of osmium containing guanidine-derived ligands.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13601
_journal_page_last               13617
_journal_paper_doi               10.1039/d0dt02713h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C31 H36 Cl N4 Os, F6 Sb, 1.5(C H4 O)'
_chemical_formula_sum            'C32.5 H42 Cl F6 N4 O1.5 Os Sb'
_chemical_formula_weight         974.10
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Fourier difference synthesis'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                92.1850(10)
_cell_angle_beta                 93.7980(10)
_cell_angle_gamma                110.5430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8413(6)
_cell_length_b                   11.1473(6)
_cell_length_c                   15.2059(6)
_cell_measurement_reflns_used    7899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.160
_cell_measurement_theta_min      2.250
_cell_volume                     1713.31(15)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'narrow \w frames'
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21006
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.621
_diffrn_reflns_theta_min         2.255
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.638
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_correction_T_min  0.5093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       plate
_exptl_crystal_F_000             950
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0276P)^2^+1.3390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7033
_reflns_number_total             7990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02713h2.cif
_cod_data_source_block           cmpnd_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct method' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7705482--7705488.cif.
;
_cod_original_formula_sum        'C32.50 H42 Cl F6 N4 O1.50 Os Sb'
_cod_database_code               7705482
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              68563
_shelx_fab_checksum              31716