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_7042074
_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
'C42.89 H65.68 Al Cl0.11 N4 P3 Rh, 0.5(C6 H6)'
_chemical_formula_sum            'C42.89 H65.68 Al Cl0.11 N4 P3 Rh'
_chemical_formula_weight         863.98
_chemical_name_common            16250_Complex-1-CH3
_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   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                67.2469(11)
_cell_angle_beta                 81.6400(11)
_cell_angle_gamma                76.0822(12)
_cell_formula_units_Z            2
_cell_length_a                   12.3599(3)
_cell_length_b                   13.5401(3)
_cell_length_c                   14.2951(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.5765
_cell_measurement_theta_min      3.3585
_cell_volume                     2137.74(9)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, 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      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Photon-II CMOS'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44289
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.637
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'I\^I1/4S Cu-microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene, Pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.096
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.6210
_refine_diff_density_max         3.302
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0641P)^2^+4.0068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7966
_reflns_number_total             8694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04769f2.cif
_cod_data_source_block           16250_Complex-1-CH3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7042071--7042076.cif.
;
_cod_database_code               7042074
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.446
_shelx_estimated_absorpt_t_max   0.655
_shelx_res_checksum              74283