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_7042075
_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 H60 Cl Ga N4 P3 Rh, 0.5(C6 H6)'
_chemical_formula_sum            'C42 H63 Cl Ga N4 P3 Rh'
_chemical_formula_weight         924.95
_chemical_name_common            14251_Complex-2-Cl
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 108.349(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2670(19)
_cell_length_b                   26.703(4)
_cell_length_c                   13.837(2)
_cell_measurement_reflns_used    3317
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.612
_cell_measurement_theta_min      2.175
_cell_volume                     4302.1(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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_R_equivalents  0.1119
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.782
_diffrn_reflns_theta_min         1.525
_diffrn_source                   'normal focus-sealed tube'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene, Hexanes'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.5464
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8209
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0440P)^2^+0.7508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5294
_reflns_number_total             8209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04769f2.cif
_cod_data_source_block           14251_Complex-2-Cl
_cod_depositor_comments
'Adding full bibliography for 7042071--7042076.cif.'
_cod_original_cell_volume        4302.0(12)
_cod_database_code               7042075
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.711
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              17073