A new supramolecular bonding motif involving NH bonds of ammonium salts and macrocycles derived from platinum corners and butadiynediyl linkers
Collins, Brenna K.; Bhuvanesh, Nattamai; Gladysz, John A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02680E

data_7711524
_publ_section_title
;
 A new supramolecular bonding motif involving NH bonds of ammonium salts
 and macrocycles derived from platinum corners and butadiynediyl linkers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02680E
_journal_year                    2022
_chemical_formula_moiety
'C140 H136 P8 Pt4, 0.14(Pt), I, 3.75(C H Cl3), C6 H12 N, 2.83(C7 H8)'
_chemical_formula_sum            'C169.56 H174.39 Cl11.25 I N P8 Pt4.14'
_chemical_formula_weight         3807.35
_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
_audit_creation_date             2022-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-30 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.217(3)
_cell_angle_beta                 76.791(3)
_cell_angle_gamma                71.491(3)
_cell_formula_units_Z            2
_cell_length_a                   18.8201(16)
_cell_length_b                   19.0800(15)
_cell_length_c                   26.635(2)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.308
_cell_volume                     8761.4(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            492199
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.749
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  0.1864
_exptl_absorpt_correction_T_min  0.1313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1265 before and 0.0601 after correction.
The Ratio of minimum to maximum transmission is 0.7044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       needle
_exptl_crystal_F_000             3772
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.024
_refine_diff_density_max         4.522
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1773
_refine_ls_number_reflns         40243
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+12.1912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31456
_reflns_number_total             40243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02680e2.cif
_cod_data_source_block           bciv103_sq
_cod_original_cell_volume        8761.3(13)
_cod_database_code               7711524
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.617
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1A-C1H \\sim C1A-C1D
 with sigma of 0.04
 C1B-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1H \\sim C1H-C1B
 with sigma of 0.02
 C1B-C1G \\sim C1B-C1E \\sim C1H-C1F \\sim C1D-C1H \\sim C1E-C1G \\sim C1D-C1F
 with sigma of 0.04
 C71S-C72S \\sim C72S-C73S \\sim C73S-C74S \\sim C74S-C75S \\sim C75S-C76S
\\sim C76S-C71S
 with sigma of 0.02
 C77S-C76S \\sim C77S-C72S
 with sigma of 0.04
 C71S-C75S \\sim C71S-C73S \\sim C76S-C74S \\sim C72S-C76S \\sim C73S-C75S
\\sim C72S-C74S
 with sigma of 0.04
3. Restrained planarity
 C1A, C1B, C1D, C1E, C1F, C1G, C1H
 with sigma of 0.1
 C71S, C72S, C73S, C74S, C75S, C76S, C77S
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1D \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C71S \\sim C72S \\sim C73S \\sim C74S \\sim C75S \\sim C76S \\sim C77S: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
5. Rigid body (RIGU) restrains
 C1A, C1B, C1D, C1E, C1F, C1G, C1H
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C71S, C72S, C73S, C74S, C75S, C76S, C77S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Others
 Fixed Sof: Pt5(0.11) Pt6(0.03) Cl11(0.83) Cl12(0.83) Cl13(0.83) C14S(0.83)
 H14S(0.83) Cl41(0.92) Cl42(0.92) Cl43(0.92) C44S(0.92) H44S(0.92) C77S(0.83)
 H77A(0.83) H77B(0.83) H77C(0.83) C71S(0.83) C72S(0.83) H72S(0.83) C73S(0.83)
 H73S(0.83) C74S(0.83) H74S(0.83) C75S(0.83) H75S(0.83) C76S(0.83) H76S(0.83)
7.a Free rotating group:
 C1A(C1B,C1D,C1E,C1F,C1G,C1H), C77S(C71S,C72S,C73S,C74S,C75S,C76S)
7.b Ternary CH refined with riding coordinates:
 C14S(H14S), C24S(H24S), C34S(H34S), C44S(H44S)
7.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,
 H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B),
 C33(H33A,H33B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B),
  C41(H41A,H41B), C43(H43A,H43B), N4C(H4CA,H4CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB)
7.d Aromatic/amide H refined with riding coordinates:
 C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71),
 C72(H72), C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
  C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89),
 C90(H90), C91(H91), C92(H92), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
  C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116), C118(H118), C119(H119), C120(H120),
 C121(H121), C122(H122), C124(H124), C125(H125), C126(H126), C127(H127),
 C128(H128), C130(H130), C131(H131), C132(H132), C133(H133), C134(H134),
 C136(H136), C137(H137), C138(H138), C139(H139), C140(H140), C2C(H2C), C6C(H6C),
  C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1H(H1H), C52S(H52S), C53S(H53S),
 C54S(H54S), C55S(H55S), C56S(H56S), C72S(H72S), C73S(H73S), C74S(H74S),
 C75S(H75S), C76S(H76S)
7.e X=CH2 refined with riding coordinates:
 C1C(H1CA,H1CB), C7C(H7CA,H7CB)
7.f Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C1A(H1AA,H1AB,H1AC), C57S(H57A,H57B,H57C), C77S(H77A,H77B,H77C)
;
_shelx_res_checksum              92661
_shelx_hkl_checksum              29892
_shelx_fab_checksum              57749
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'