Self-Assembled Cyclophane-Type Copper(I) Complexes of 2,4,6-Tris(diphenylphosphino)-1,3,5-triazine and Their Catalytic Application.
Ananthnag, Guddekoppa S.; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic chemistry 54 (2015) 10985–10992; doi:10.1021/acs.inorgchem.5b02075

data_4346755
_publ_section_title
;
 Self-Assembled Cyclophane-Type Copper(I) Complexes of
 2,4,6-Tris(diphenylphosphino)-1,3,5-triazine and Their Catalytic
 Application.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10985
_journal_page_last               10992
_journal_paper_doi               10.1021/acs.inorgchem.5b02075
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C84 H70 Cl5 Cu3 N8 P6'
_chemical_formula_sum            'C84 H70 Cl5 Cu3 N8 P6'
_chemical_formula_weight         1745.17
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.5311(3)
_cell_length_b                   17.5311(3)
_cell_length_c                   23.1240(4)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.4855
_cell_measurement_theta_min      2.9106
_cell_volume                     6154.77(18)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2013)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2013)'
_computing_data_reduction        '<i>SAINT</i>  (Bruker, 2013)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXT</i> (Bruker AXS 2013c)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40344
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.605
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    3.893
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2013)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.926
_exptl_transmission_factor_min   0.799
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack, 2004).
;
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0528P)^2^+3.9897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                6563
_reflns_number_total             7220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02075_si_003.cif
_cod_data_source_block           MSB598_0m_a
_cod_original_cell_volume        6154.8(2)
_cod_database_code               4346755
_shelx_estimated_absorpt_t_min   0.772
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-4
_shelx_res_checksum              78591
_shelx_hkl_checksum              56140