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_7127300
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-16 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                   30.2541(5)
_cell_length_b                   30.2541(5)
_cell_length_c                   10.0134(2)
_cell_measurement_reflns_used    4676
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.3640
_cell_measurement_theta_min      4.7040
_cell_volume                     7937.4(2)
_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 (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      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.956
_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      8.00  71.00   0.50    2.95    --   42.80 -99.00-139.00  126
  2  \w     37.00 100.00   0.50    5.37    --  108.63 -99.00-139.00  126
  3  \w     44.00  71.00   0.50    5.37    --  108.63 -45.00-150.00   54
  4  \w     40.00  65.00   0.50    5.37    --  108.63 -30.00-120.00   50
  5  \w     37.00  63.00   0.50    5.37    --  108.63 -30.00 -90.00   52
  6  \w     38.00  64.00   0.50    5.37    --  108.63 -30.00 -30.00   52
  7  \w     36.00  61.00   0.50    5.37    --  108.63 -27.00 -16.00   50
  8  \w     34.00  59.00   0.50    5.37    --  108.63 -45.00 -30.00   50
  9  \w     37.00  62.00   0.50    5.37    --  108.63 -45.00 -90.00   50
 10  \w     30.00  66.00   0.50    5.37    --  108.63 -30.00-150.00   72
 11  \w     39.00  64.00   0.50    5.37    --  108.63 -30.00-180.00   50
 12  \w     34.00  75.00   0.50    5.37    --  108.63 -45.00  30.00   82
 13  \w     32.00  57.00   0.50    5.37    --  108.63 -30.00  60.00   50
 14  \w     83.00 117.00   0.50    2.95    --   42.80 125.00-180.00   68
 15  \w    -48.00 -19.00   0.50    5.37    --  -84.50  27.00-158.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0552637000
_diffrn_orient_matrix_UB_12      0.0447845000
_diffrn_orient_matrix_UB_13      -0.0081943000
_diffrn_orient_matrix_UB_21      -0.0035008000
_diffrn_orient_matrix_UB_22      0.0143756000
_diffrn_orient_matrix_UB_23      0.1457351000
_diffrn_orient_matrix_UB_31      0.0197367000
_diffrn_orient_matrix_UB_32      -0.0352888000
_diffrn_orient_matrix_UB_33      0.0486662000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8283
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.677
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74610
_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_colour_primary    orange
_exptl_crystal_density_diffrn    2.028
_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         0.944
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0308P)^2^+30.1977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3269
_reflns_number_total             3517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05349j2.cif
_cod_data_source_block           1P-cHex_100K
_cod_depositor_comments
'Adding full bibliography for 7127299--7127303.cif.'
_cod_original_cell_volume        7937.4(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7127300
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H13N3O2Pt
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C9(H9), C2(H2A), C10(H10), C5(H5), C17(H17), C14(H14), C12(H12),
 C16(H16), C15(H15), C11(H11), C3(H3), C4(H4)
;
_shelx_res_checksum              34227
_shelx_hkl_checksum              16185
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.856
_oxdiff_exptl_absorpt_empirical_full_min 0.693