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_4346752
_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_formula_moiety         'C39 H30 N3 P3'
_chemical_formula_sum            'C39 H30 N3 P3'
_chemical_formula_weight         633.57
_chemical_name_systematic
;
Tris(diphenylphosphanyl)-1,3,5-triazine
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                89.790(1)
_cell_angle_beta                 79.542(1)
_cell_angle_gamma                84.910(1)
_cell_formula_units_Z            4
_cell_length_a                   10.2469(2)
_cell_length_b                   13.8978(3)
_cell_length_c                   23.3456(4)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      72.4057
_cell_measurement_theta_min      3.7498
_cell_volume                     3256.25(11)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2014)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2014)'
_computing_data_reduction        '<i>SAINT</i>  (Bruker, 2014)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2014)'
_computing_structure_refinement  '<i>SHELXL-2014</i> (Sheldrick, 2014)'
_computing_structure_solution    '<i>SHELXT</i> (Bruker, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.945
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25575
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        72.175
_diffrn_reflns_theta_max         72.399
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.053
_exptl_transmission_factor_max   0.980
_exptl_transmission_factor_min   0.804
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0506P)^2^+0.1238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8911
_reflns_number_total             12205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02075_si_002.cif
_cod_data_source_block           MSB658a_0m_a
_cod_database_code               4346752
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.905
_shelx_res_checksum              55270
_shelx_hkl_checksum              92478