Preliminary chemical reduction for synthesizing a stable porous molecular conductor with neutral metal nodes.
Koyama, Shohei; Tanabe, Tappei; Takaishi, Shinya; Yamashita, Masahiro; Iguchi, Hiroaki; Chemical communications (Cambridge, England) 56 (2020) 13109–13112; doi:10.1039/d0cc03541f

data_7127327
_publ_section_title
;
 Preliminary chemical reduction for synthesizing a stable porous molecular
 conductor with neutral metal nodes.
;
_journal_issue                   86
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13109
_journal_page_last               13112
_journal_paper_doi               10.1039/d0cc03541f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C34 H26 Co N4 O8 0.5-, Rb0.5 0.5+, 2(C4 H9 N O)'
_chemical_formula_sum            'C42 H44 Co N6 O10 Rb0.5'
_chemical_formula_weight         894.49
_space_group_crystal_system      hexagonal
_space_group_IT_number           181
_space_group_name_Hall           'P 64 2 (0 0 2)'
_space_group_name_H-M_alt        'P 64 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-16 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.8453(7)
_cell_length_b                   19.8453(7)
_cell_length_c                   9.5591(7)
_cell_measurement_reflns_used    12480
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.8190
_cell_measurement_theta_min      2.0450
_cell_volume                     3260.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29482
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.779
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       rod
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 753 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0979P)^2^+0.9127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1706
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                2297
_reflns_number_total             3274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03541f2.cif
_cod_data_source_block           NDI-py_Coacac
_cod_depositor_comments
'Adding full bibliography for 7127326--7127327.cif.'
_cod_original_sg_symbol_Hall     'P 64 2c (0 0 -1)'
_cod_original_formula_sum        'C42 H44 Co N6 O10 Rb0.50'
_cod_database_code               7127327
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              39656