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_7127326
_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, 2(C4 H9 N O)'
_chemical_formula_sum            'C42 H44 Co N6 O10'
_chemical_formula_weight         851.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-05-16 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.416(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2874(6)
_cell_length_b                   19.8376(9)
_cell_length_c                   11.0367(6)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8510
_cell_measurement_theta_min      2.3610
_cell_volume                     2096.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.914
_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   -110.00  70.00   0.50    1.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    1.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0476974000
_diffrn_orient_matrix_UB_12      0.0040517000
_diffrn_orient_matrix_UB_13      0.0323494000
_diffrn_orient_matrix_UB_21      0.0541696000
_diffrn_orient_matrix_UB_22      -0.0071122000
_diffrn_orient_matrix_UB_23      0.0603817000
_diffrn_orient_matrix_UB_31      0.0166826000
_diffrn_orient_matrix_UB_32      0.0348058000
_diffrn_orient_matrix_UB_33      0.0086363000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18560
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.742
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.6783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             5976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03541f2.cif
_cod_data_source_block           coacac_dpndi
_cod_depositor_comments
'Adding full bibliography for 7127326--7127327.cif.'
_cod_database_code               7127326
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H00W)=Sof(H00X)=Sof(H00Y)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(N00U)=
 Sof(C00V)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(C00Q)=Sof(H00L)=Sof(H00M)=Sof(H00P)=Sof(C00R)=Sof(H00Q)=Sof(H00R)=
 Sof(H00S)=Sof(H00T)=Sof(H00U)=Sof(H00V)=Sof(N00T)=Sof(C00U)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00G(H00G), C00H(H00H), C00K(H00K), C00N(H00N),
 C00O(H00O)
3.b Idealised Me refined as rotating group:
 C00J(H00A,H00B,H00C), C00P(H00E,H00I,H00J), C00Q(H00L,H00M,H00P), C00R(H00Q,
 H00R,H00S), C00S(H00T,H00U,H00V), C00S(H00W,H00X,H00Y), C1(H1A,H1B,H1C),
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              43221
_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 3.258
_oxdiff_exptl_absorpt_empirical_full_min 0.514