Structure and dynamic NMR behavior of rhodium complexes supported by Lewis acidic group 13 metallatranes.
Moore, James T.; Smith, Nicholas E.; Lu, Connie C.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5689–5701; doi:10.1039/c6dt04769f

data_7042073
_publ_section_title
;
 Structure and dynamic NMR behavior of rhodium complexes supported by
 Lewis acidic group 13 metallatranes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5689
_journal_page_last               5701
_journal_paper_doi               10.1039/c6dt04769f
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C39 H61 Al N4 P3 Rh, 0.5(C6 H6)'
_chemical_formula_sum            'C42 H64 Al N4 P3 Rh'
_chemical_formula_weight         847.77
_chemical_name_common            16232_Complex_1-H
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-16 deposited with the CCDC.
2017-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                69.082(7)
_cell_angle_beta                 77.640(7)
_cell_angle_gamma                82.728(7)
_cell_formula_units_Z            2
_cell_length_a                   11.611(7)
_cell_length_b                   14.168(8)
_cell_length_c                   14.280(8)
_cell_measurement_reflns_used    3622
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.224
_cell_measurement_theta_min      2.2502
_cell_volume                     2140(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX2, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-2014 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8104
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.757
_diffrn_reflns_theta_min         1.541
_diffrn_source                   'normal focus-sealed tube'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2012/1, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             894
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene, hexanes'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.745262
_exptl_transmission_factor_min   0.592620
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6320
_reflns_number_total             8104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04769f2.cif
_cod_data_source_block           16232_Complex_1-H
_cod_depositor_comments
'Adding full bibliography for 7042071--7042076.cif.'
_cod_database_code               7042073
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.946
_exptl_absorpt_special_details
'The crystal under investigation was found to be non-merohedrally twinned. Orientation matrices for the two components were identified using the program Cell_Now. The two components were related by a 180 degree rotation around the real and reciprocal axes of b and c. The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1, resulting in a BASF value of 0.151.'
_shelx_res_checksum              74838