Rylene- and diaza-rylene-derived cobalt clusters for solid-state pyrolysis towards undoped and N-doped carbon nanoparticles
Werner, Simon; Vollgraff, Tobias; Sundermeyer, Jörg; Dalton Transactions  (2021) –; doi:10.1039/D1DT02276H

data_7708440
_publ_section_title
;
 Rylene- and diaza-rylene-derived cobalt clusters for solid-state
 pyrolysis towards undoped and N-doped carbon nanoparticles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02276H
_journal_year                    2021
_chemical_formula_moiety         'C68 H44 Co8 N2 O24 Si4, 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H48 Cl4 Co8 N2 O24 Si4'
_chemical_formula_weight         2026.70
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.762(19)
_cell_angle_beta                 99.807(18)
_cell_angle_gamma                94.55(3)
_cell_formula_units_Z            1
_cell_length_a                   8.276(7)
_cell_length_b                   14.505(12)
_cell_length_c                   17.743(14)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0949
_cell_measurement_theta_min      2.3913
_cell_volume                     2040(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics
'DIAMOND 4 (H. Putz, K. Brandenburg, Crystal Impact GbR, Kreuzherrenstr. 102, 53227 Bonn, Germany)'
_computing_publication_material
; 
'WinGX 2014.1 (L.J. Farrugia, J. Appl. Cryst. 2012, 45, 849-854)'
'enCIFer (F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler, J. Appl. Cryst. 2004, 37, 335-338.)'
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.253
_diffrn_reflns_theta_min         2.389
_diffrn_source                   'I\mS Microfocus Source'
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         7323
_refine_ls_number_restraints     490
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0471P)^2^+5.4523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             7323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02276h2.cif
_cod_data_source_block           swp60_0m_a
_cod_database_code               7708440
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.516
_shelx_estimated_absorpt_t_max   0.865
_shelx_res_checksum              83268