Nitroxyl radical-containing flexible porous coordination polymer for controllable size-aelective aerobic oxidation of alcohols.
Wang, Ping; Xue, Ziqian; Ken-Ichi, Otake; Kitagawa, Susumu; Chemical communications (Cambridge, England) 58 (2022) 9026–9029; doi:10.1039/d2cc02772k

data_7130648
_publ_section_title
;
 Nitroxyl radical-containing flexible porous coordination polymer for
 controllable size-aelective aerobic oxidation of alcohols.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9026
_journal_page_last               9029
_journal_paper_doi               10.1039/d2cc02772k
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C86 H87 N8 O14 Zn2, +5[C7H8]'
_chemical_formula_sum            'C121 H127 N8 O14 Zn2'
_chemical_formula_weight         2048.17
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.038(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.1988(9)
_cell_length_b                   28.6120(9)
_cell_length_c                   36.1248(10)
_cell_measurement_reflns_used    17083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9800
_cell_measurement_theta_min      2.8230
_cell_volume                     26381.1(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            75159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.873
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.799
_exptl_crystal_description       block
_exptl_crystal_F_000             6648
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         25815
_refine_ls_number_restraints     797
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1991P)^2^+8.1132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2933
_refine_ls_wR_factor_ref         0.3228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14958
_reflns_number_total             25815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02772k2.cif
_cod_data_source_block           DT-PCP-toluene
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7130648
_shelx_shelxl_version_number     2018/1
_oxdiff_exptl_absorpt_empirical_full_min 0.774
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              11921
_shelx_hkl_checksum              86958
_shelx_fab_checksum              24958