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_7711523
_publ_section_title
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 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         'C132 H120 P8 Pt4, Cl, C4 H10 N O'
_chemical_formula_sum            'C136 H130 Cl N O P8 Pt4'
_chemical_formula_weight         2857.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-02
_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                90
_cell_angle_beta                 90.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3077(14)
_cell_length_b                   26.3723(14)
_cell_length_c                   21.7373(12)
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      70.111
_cell_measurement_theta_min      3.162
_cell_volume                     14508.0(14)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_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            142334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.258
_diffrn_reflns_theta_min         2.420
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.372
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.1542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1233 before and 0.0715 after correction.
The Ratio of minimum to maximum transmission is 0.4015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.045
_refine_diff_density_max         8.094
_refine_diff_density_min         -2.333
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         13825
_refine_ls_number_restraints     1084
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0971P)^2^+204.9627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12912
_reflns_number_total             13825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02680e2.cif
_cod_data_source_block           bciv28
_cod_database_code               7711523
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.462
_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
 O1M-C3M \\sim O1M-C2M \\sim N1M-C1M \\sim N1M-C4M
 with sigma of 0.005
 C2M-C1M \\sim C4M-C3M
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Others
 Fixed Sof: Cl1(0.5) C1M(0.5) H1MA(0.5) H1MB(0.5) C2M(0.5) H2MA(0.5) H2MB(0.5)
 O1M(0.5) C3M(0.5) H3MA(0.5) H3MB(0.5) C4M(0.5) H4MA(0.5) H4MB(0.5) N1M(0.5)
 H1MC(0.5) H1MD(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1M(H1MA,H1MB), C2M(H2MA,H2MB), C3M(H3MA,H3MB), C4M(H4MA,H4MB), N1M(H1MC,
 H1MD), C7(H7A,H7B), C11(H11A,H11B), C7(H7A,H7B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C2(H2), C3(H3), C4(H4), C5(H5),
 C6(H6), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C1(H1), C2(H2), C3(H3), C4(H4),
  C5(H5), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C1(H1), C2(H2), C3(H3),
 C4(H4), C5(H5), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C1(H1), C2(H2), C3(H3),
  C4(H4), C6(H6)
6.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,
 C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,
 C5,C6)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49235
_shelx_hkl_checksum              49382
_shelx_fab_checksum              92161
_olex2_submission_special_instructions 'No special instructions were received'