Diaminohexopyranosides as Ligands in Half-Sandwich Ruthenium(II), Rhodium(III), and Iridium(III) Complexes
Böge, Matthias; Fowelin, Christian; Bednarski, Patrick; Heck, Jürgen; Organometallics 34 (2015) 1507–; doi:10.1021/om5013117

data_4085690
_publ_section_title
;
 Diaminohexopyranosides as Ligands in Half-Sandwich Ruthenium(II),
 Rhodium(III), and Iridium(III) Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1507
_journal_paper_doi               10.1021/om5013117
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration known
_chemical_formula_moiety
'C24 H35 Cl N2 O4 Rh, C24 H35 Cl N2 O4 Rh, C24 H35 Cl N2 O4 Rh, B F4, B F4, Cl, H2 O'
_chemical_formula_sum            'C72 H107 B2 Cl4 F8 N6 O13 Rh3'
_chemical_formula_weight         1888.78
_chemical_name_systematic
;
Tris{[T-4-R]-chlorido(methyl 
4,6-O-benzylidene-2,3-diamino-2,3-dideoxy-alpha-D-mannopyranoside)pentamethyl-pentahapto-cyclopentadienylrhodium(III)} 
bistetrafluoridoborate chloride water
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'Difference Fourier'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.9780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9435(4)
_cell_length_b                   23.2329(8)
_cell_length_c                   16.4422(6)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.17
_cell_volume                     4386.2(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 1998)'
_computing_data_collection       'SMART (Bruker AXS, 1998)'
_computing_data_reduction        'SAINT (Bruker AXS, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            120914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.000
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'Incoatec microfocus'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.078
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 11690 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         32735
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0363P)^2^+0.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                27800
_reflns_number_total             32735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5013117_si_001.cif
_cod_data_source_block           39
_cod_depositor_comments
;Adding full bibliography for 4085684--4085692.cif.

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4085690
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2013-4
_shelx_res_checksum              11256
_shelx_hkl_checksum              79917