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_7043710
_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            'C90 H112 F12 N10 O27 Rh4 S4'
_chemical_formula_weight         2533.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                109.857(2)
_cell_angle_beta                 91.607(2)
_cell_angle_gamma                96.139(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3538(17)
_cell_length_b                   17.894(2)
_cell_length_c                   20.376(2)
_cell_measurement_reflns_used    3306
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.30
_cell_volume                     5222.7(10)
_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  0.1673
_diffrn_reflns_av_unetI/netI     0.2551
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32624
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.219
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             2580
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (four methanol and one water molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.453
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         18395
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8090
_reflns_number_total             18395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02186k2.cif
_cod_data_source_block           mo_60506c
_cod_original_cell_volume        5222.8(10)
_cod_database_code               7043710
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.932
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              97497