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_7705487
_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         'C39 H44 Cl N3 Os P, F6 Sb'
_chemical_formula_sum            'C39 H44 Cl F6 N3 Os P Sb'
_chemical_formula_weight         1047.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9424(4)
_cell_length_b                   13.4216(5)
_cell_length_c                   25.9506(10)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.393
_cell_measurement_theta_min      2.435
_cell_volume                     3811.2(2)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0331
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.777
_diffrn_reflns_theta_min         1.569
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.214
_exptl_absorpt_correction_T_max  0.5016
_exptl_absorpt_correction_T_min  0.3736
_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    1.825
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.146
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 4470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         10435
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+2.7668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0411
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                10312
_reflns_number_total             10435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02713h2.cif
_cod_data_source_block           cmpnd_2
_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_database_code               7705487
_shelxl_version_number           2014-3
_shelx_res_checksum              33269