Postsynthetic modifications of [2,2,2-(H)(PPh3)2-closo-2,1-RhSB8H8] with Lewis bases: cluster modular tuning.
Luaces, Susana; Passarelli, Vincenzo; Artigas, María José; Lahoz, Fernando J.; Oro, Luis A.; Macías, Ramón; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8622–8636; doi:10.1039/c6dt00856a

data_7039044
_publ_section_title
;
 Postsynthetic modifications of [2,2,2-(H)(PPh3)2-closo-2,1-RhSB8H8] with
 Lewis bases: cluster modular tuning.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8622
_journal_page_last               8636
_journal_paper_doi               10.1039/c6dt00856a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C42 H46 B8 N1 P2 Rh1 S1), C H2 Cl2'
_chemical_formula_sum            'C85 H94 B16 Cl2 N2 P4 Rh2 S2'
_chemical_formula_weight         1781.30
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-29 deposited with the CCDC.
2016-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                79.2790(10)
_cell_angle_beta                 75.5540(10)
_cell_angle_gamma                65.0620(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2617(12)
_cell_length_b                   13.1022(14)
_cell_length_c                   16.6998(18)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.306
_cell_measurement_theta_min      2.178
_cell_volume                     2154.5(4)
_computing_cell_refinement       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ENCIFER
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow 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  0.0323
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50593
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.672
_diffrn_reflns_theta_min         1.265
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.909
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         10360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0308P)^2^+2.4203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9066
_reflns_number_total             10360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00856a2.cif
_cod_data_source_block           VPX31DS
_cod_depositor_comments
'Adding full bibliography for 7039041--7039044.cif.'
_cod_database_code               7039044
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              52475