Stepwise construction of discrete parallelogram- and prism-shaped organometallic architectures based on half-sandwich rhodium fragments
Jin, Guo-Xin; Gao, Wen-Xi; Lin, Yue-Jian; Dalton Trans.  (2017) –; doi:10.1039/C7DT02186K

data_7043712
_publ_section_title
;
 Stepwise construction of discrete parallelogram- and prism-shaped
 organometallic architectures based on half-sandwich rhodium fragments
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02186K
_journal_year                    2017
_chemical_formula_sum            'C120 H146 F18 N12 O33 Rh6 S6'
_chemical_formula_weight         3436.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.754(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.867(5)
_cell_length_b                   26.493(6)
_cell_length_c                   27.213(6)
_cell_measurement_reflns_used    4378
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.39
_cell_measurement_theta_min      2.20
_cell_volume                     15096(6)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0929
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49051
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.240
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       block
_exptl_crystal_F_000             6968
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (three triflate anions, two methanol 
 and one water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         14808
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7283
_reflns_number_total             14808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02186k2.cif
_cod_data_source_block           mo_60514a
_cod_database_code               7043712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.867
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              84967