Formation of Planar Chiral Platinum Triangles via Pillar[5]arene for Circularly Polarized Luminescence.
Zhu, Huangtianzhi; Li, Qi; Shi, Bingbing; Xing, Hao; Sun, Yan; Lu, Shuai; Shangguan, Liqing; Li, Xiaopeng; Huang, Feihe; Stang, Peter J.; Journal of the American Chemical Society 142 (2020) 17340–17345; doi:10.1021/jacs.0c09598

data_4135272
_publ_section_title
;
 Formation of Planar Chiral Platinum Triangles via Pillar[5]arene for
 Circularly Polarized Luminescence.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17340
_journal_page_last               17345
_journal_paper_doi               10.1021/jacs.0c09598
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '1.5(C H Cl3), C65 H60 N2 O8, C5 H12'
_chemical_formula_sum            'C71.5 H73.5 Cl4.5 N2 O8'
_chemical_formula_weight         1248.34
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1923(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9642(2)
_cell_length_b                   26.3927(4)
_cell_length_c                   21.6924(3)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.86
_cell_measurement_theta_min      3.41
_cell_volume                     6849.72(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            89724
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.919
_diffrn_reflns_theta_min         3.214
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1136 before and 0.0646 after correction. The Ratio of minimum to maximum transmission is 0.7983. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 9508 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.072(5)
_refine_ls_extinction_coef       0.0033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1570
_refine_ls_number_reflns         25961
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0998P)^2^+4.4567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                22954
_reflns_number_total             25961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c09598_si_001.cif
_cod_data_source_block           191025zhtz_0m
_cod_depositor_comments
'Adding full bibliography for 4135272--4135273.cif.'
_cod_original_formula_sum        'C71.50 H73.50 Cl4.50 N2 O8'
_cod_database_code               4135272
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C138-C134
 1.53 with sigma of 0.02
 C138-C134 = C135-C134 = C136-C135 = C137-C136
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C137 \\sim C136 \\sim C135 \\sim C134 \\sim C138: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C20(H20A,H20B), C25(H25A,H25B), C34(H34A,H34B), C43(H43A,
 H43B), C76(H76A,H76B), C85(H85A,H85B), C90(H90A,H90B), C99(H99A,H99B),
 C108(H10G,H10H), C134(H13D,H13E), C135(H13F,H13G), C136(H13H,H13I), C139(H13P,
 H13Q), C140(H14D,H14E), C141(H14F,H14G)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C15(H15), C19(H19), C23(H23), C29(H29), C33(H33), C38(H38),
 C42(H42), C45(H45), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56), C58(H58), C59(H59), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66), C67(H67), C71(H71), C75(H75), C80(H80), C84(H84), C88(H88),
  C94(H94), C98(H98), C103(H103), C107(H107), C110(H110), C112(H112),
 C113(H113), C116(H116), C117(H117), C118(H118), C119(H119), C120(H120),
 C121(H121), C123(H123), C124(H124), C127(H127), C128(H128), C129(H129),
 C130(H130), C131(H131), C132(H132)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C68(H68A,
 H68B,H68C), C73(H73A,H73B,H73C), C79(H79A,H79B,H79C), C83(H83A,H83B,H83C),
 C93(H93A,H93B,H93C), C97(H97A,H97B,H97C), C102(H10A,H10B,H10C), C106(H10D,H10E,
 H10F), C133(H13A,H13B,H13C), C137(H13J,H13K,H13L), C138(H13M,H13N,H13O),
 C142(H14H,H14I,H14J), C143(H14K,H14L,H14M)
;
_shelx_res_checksum              23155
_shelx_hkl_checksum              2829
_shelx_fab_checksum              5190
_olex2_submission_special_instructions 'No special instructions were received'