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_4346754
_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         'C79 H62 Br3 Cl Cu3 N6 P6'
_chemical_formula_sum            'C79 H62 Br3 Cl Cu3 N6 P6'
_chemical_formula_weight         1746.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.724(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.192(4)
_cell_length_b                   18.254(4)
_cell_length_c                   24.392(5)
_cell_measurement_reflns_used    9068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      0.90
_cell_volume                     7495(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56156
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.6189
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3476
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0077P)^2^+25.8770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                10269
_reflns_number_total             13164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02075_si_004.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               4346754
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H72(0.021) H34(0.025) H16(0.028) H68(0.023) H39(0.028) H75(0.026)
 H20(0.022) H66(0.026) H9(0.033) H78(0.018) H46(0.025) H77(0.024) H33(0.026)
 H22(0.024) H57(0.032) H47(0.026) H26(0.024) H14(0.019) H62(0.026) H24(0.022)
 H23(0.024) H63(0.026) H56(0.028) H54(0.023) H74(0.018) H59(0.027) H36(0.025)
 H48(0.018) H45(0.028) H38(0.02) H44(0.023) H79A(0.053) H79B(0.053) H64(0.026)
 H60(0.023) H17(0.026) H71(0.023) H42(0.028) H69(0.028) H53(0.031) H12(0.029)
 H40(0.031) H15(0.024) H21(0.029) H32(0.024) H8(0.022) H70(0.027) H18(0.021)
 H65(0.026) H76(0.024) H58(0.028) H41(0.042) H52(0.031) H30(0.034) H35(0.03)
 H11(0.037) H27(0.031) H10(0.037) H28(0.042) H51(0.037) H50(0.029) H29(0.056)
 Fixed X: H72(0.4136) H34(0.8399) H16(0.7599) H68(0.6466) H39(0.955)
 H75(0.6629) H20(0.3868) H66(0.236) H9(0.3488) H78(0.4335) H46(0.5042)
 H77(0.423) H33(0.8127) H22(0.5638) H57(0.0802) H47(0.5229) H26(0.4254)
 H14(0.5731) H62(0.2784) H24(0.6083) H23(0.6518) H63(0.2371) H56(0.1941)
 H54(0.3006) H74(0.6736) H59(0.0764) H36(0.7654) H48(0.4927) H45(0.4605)
 H38(0.8757) H44(0.4282) H79A(0.5248) H79B(0.4352) H64(0.1985) H60(0.1892)
 H17(0.7316) H71(0.3832) H42(0.6894) H69(0.6163) H53(0.1669) H12(0.3396)
 H40(0.8979) H15(0.6811) H21(0.433) H32(0.7632) H8(0.4644) H70(0.4851)
 H18(0.6218) H65(0.1969) H76(0.5368) H58(0.0248) H41(0.7658) H52(0.0994)
 H30(0.589) H35(0.816) H11(0.224) H27(0.4812) H10(0.2278) H28(0.589)
 H51(0.1643) H50(0.2975) H29(0.6446)
 Fixed Y: H72(0.544) H34(0.9061) H16(0.7918) H68(0.5834) H39(0.6071)
 H75(0.2776) H20(0.9378) H66(0.7444) H9(0.8489) H78(0.4232) H46(0.1745)
 H77(0.2968) H33(0.8187) H22(1.0446) H57(0.4906) H47(0.2303) H26(0.7356)
 H14(0.7947) H62(0.5278) H24(0.8499) H23(0.9506) H63(0.5057) H56(0.5241)
 H54(0.5218) H74(0.4048) H59(0.6878) H36(0.7656) H48(0.3534) H45(0.2451)
 H38(0.6577) H44(0.368) H79A(0.9742) H79B(0.9701) H64(0.6033) H60(0.7235)
 H17(0.6719) H71(0.5807) H42(0.5361) H69(0.6164) H53(0.4999) H12(0.6405)
 H40(0.5259) H15(0.8545) H21(1.0391) H32(0.7038) H8(0.7843) H70(0.6149)
 H18(0.6126) H65(0.7213) H76(0.2243) H58(0.5709) H41(0.4918) H52(0.4114)
 H30(0.8839) H35(0.8793) H11(0.7067) H27(0.7376) H10(0.8079) H28(0.8125)
 H51(0.3534) H50(0.3761) H29(0.8846)
 Fixed Z: H72(0.8801) H34(0.8485) H16(0.5236) H68(0.9425) H39(0.6973)
 H75(0.8703) H20(0.7103) H66(0.8263) H9(0.4758) H78(0.8326) H46(0.6712)
 H77(0.8433) H33(0.9108) H22(0.6569) H57(0.6551) H47(0.5888) H26(0.8562)
 H14(0.5994) H62(0.8099) H24(0.7343) H23(0.6908) H63(0.8951) H56(0.7204)
 H54(0.5328) H74(0.8599) H59(0.5805) H36(0.7202) H48(0.5718) H45(0.739)
 H38(0.7548) H44(0.7225) H79A(0.5554) H79B(0.5199) H64(0.9448) H60(0.6471)
 H17(0.495) H71(0.965) H42(0.6767) H69(1.0278) H53(0.4987) H12(0.5854)
 H40(0.6257) H15(0.576) H21(0.6673) H32(0.879) H8(0.51) H70(1.0393) H18(0.5175)
 H65(0.911) H76(0.8627) H58(0.5844) H41(0.6158) H52(0.5394) H30(0.8299)
 H35(0.7521) H11(0.5502) H27(0.9524) H10(0.4932) H28(0.9865) H51(0.6209)
 H50(0.6579) H29(0.9261)
;
_shelx_res_checksum              15036