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_7042071
_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         '2(C39 H61 Ga N4 P3 Rh), C6 H6'
_chemical_formula_sum            'C42 H64 Ga N4 P3 Rh'
_chemical_formula_weight         890.51
_chemical_name_common            16212_Complex-2-H
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                90
_cell_angle_beta                 106.028(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.300(2)
_cell_length_b                   27.928(5)
_cell_length_c                   12.784(3)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.0575
_cell_measurement_theta_min      2.208
_cell_volume                     4220.8(14)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEXII, 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 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.228
_diffrn_reflns_theta_min         1.458
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene, Hexanes'
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.191
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6725
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 6574 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         18804
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0098P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                16031
_reflns_number_total             18804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04769f2.cif
_cod_data_source_block           16212a_Complex-2-H
_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               7042071
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.806
_shelx_res_checksum              51253