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_4346753
_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         'C80 H63 Cu3 I3 N7 P6, C2 H3 N'
_chemical_formula_sum            'C82 H66 Cu3 I3 N8 P6'
_chemical_formula_weight         1920.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.260(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.298(3)
_cell_length_b                   27.696(6)
_cell_length_c                   21.440(5)
_cell_measurement_reflns_used    9641
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      29.3460
_cell_measurement_theta_min      2.4017
_cell_volume                     7814(3)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2015)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2010)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2015)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2015)'
_computing_structure_refinement  '<i>SHELXL</i> (Sheldrick, 2015a)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            71809
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         29.434
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.133
_exptl_transmission_factor_max   0.773
_exptl_transmission_factor_min   0.555
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 8648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   -0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         20283
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.8116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                19328
_reflns_number_total             20283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02075_si_005.cif
_cod_data_source_block           MSB557_0m_a
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4346753
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.761
_shelx_res_checksum              43657
_shelx_hkl_checksum              66867