A covalent deprotection strategy for assembling supramolecular coordination polymers from metal-organic cages.
Schneider, Matthew L.; Linder-Patton, Oliver M; Bloch, Witold M.; Chemical communications (Cambridge, England) 56 (2020) 12969–12972; doi:10.1039/d0cc05349j

data_7127303
_publ_section_title
;
 A covalent deprotection strategy for assembling supramolecular
 coordination polymers from metal-organic cages.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12969
_journal_page_last               12972
_journal_paper_doi               10.1039/d0cc05349j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C19 H13 N3 O2 Pt, C2 H4'
_chemical_formula_sum            'C21 H17 N3 O2 Pt'
_chemical_formula_weight         538.47
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   30.2896(3)
_cell_length_b                   30.2896(3)
_cell_length_c                   10.05700(10)
_cell_measurement_reflns_used    6467
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.0840
_cell_measurement_theta_min      2.9080
_cell_volume                     7990.72(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  46.00   0.50    5.23    --   46.37 -68.00  15.00  126
  2  \w     36.00  68.00   0.50   19.22    --  108.56 -37.00   0.00   64
  3  \w     41.00  68.00   0.50   19.22    --  108.56 -19.00 -60.00   54
  4  \w     42.00  68.00   0.50   19.22    --  108.56 -37.00 -60.00   52
  5  \w     34.00  65.00   0.50   19.22    --  108.56 -19.00 -90.00   62
  6  \w     35.00  63.00   0.50   19.22    --  108.56 -37.00-150.00   56
  7  \w     34.00  60.00   0.50   19.22    --  108.56 -19.00-150.00   52
  8  \w     40.00  69.00   0.50   19.22    --  108.56 -37.00-180.00   58
  9  \w    139.00 166.00   0.50   19.22    --  108.56  61.00   9.00   54
 10  \w     99.00 133.00   0.50   19.22    --  108.56  61.00   9.00   68
 11  \w     73.00 112.00   0.50    5.23    --   46.37 125.00   0.00   78
 12  \w     33.00  60.00   0.50   19.22    --  108.56 -19.00  60.00   54
 13  \w     36.00  63.00   0.50   19.22    --  108.56 -37.00  60.00   54
 14  \w     35.00  69.00   0.50   19.22    --  108.56 -37.00  30.00   68
 15  \w    -73.00 -48.00   0.50   19.22    --  -84.50  61.00   9.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8545
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.361
_diffrn_reflns_theta_min         2.918
_exptl_absorpt_coefficient_mu    14.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       needle
_exptl_crystal_F_000             4644
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+15.8748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             3584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05349j2.cif
_cod_data_source_block           1P-cHex
_cod_depositor_comments
'Adding full bibliography for 7127299--7127303.cif.'
_cod_original_cell_volume        7990.72(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7127303
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H13N3O2Pt
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.522
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C21B-C21B_$1
 2.515 with sigma of 0.04
 C21A-C21A_$1
 2.515 with sigma of 0.04
 C20B-C20B_$1
 2.515 with sigma of 0.04
 C20A-C20A_$1
 2.515 with sigma of 0.04
 C20B-C21B \\sim C21B-C20B_$1 \\sim C20A-C21A \\sim C21A-C20A_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20A \\sim C21A \\sim C20B \\sim C21B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C20A, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(1)
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C20B(H20A,H20B), C21B(H21A,H21B), C20A(H20C,H20D), C21A(H21C,H21D)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C17(H17), C12(H12), C9(H9), C10(H10), C14(H14), C15(H15),
 C5(H5), C3(H3), C16(H16), C11(H11), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;