One-dimensional DABCO hydrogen-bonding chain in a hexagonal channel of magnetic [Ni(dmit)<sub>2</sub>].
Li, Simin; Takahashi, Kiyonori; Hisaki, Ichiro; Kokado, Kenta; Nakamura, Takayoshi; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16772–16777; doi:10.1039/d0dt03386c

data_7705859
_publ_section_title
;
 One-dimensional DABCO hydrogen-bonding chain in a hexagonal channel of
 magnetic [Ni(dmit)<sub>2</sub>].
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16772
_journal_page_last               16777
_journal_paper_doi               10.1039/d0dt03386c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'9(C6 Ni S10), 9(C6 H13 N2), (C6 H12 N2), 6(C2 H3 N)'
_chemical_formula_sum            'C126 H147 N26 Ni9 S90'
_chemical_formula_weight         5440.49
_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     dual
_audit_creation_date             2020-07-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-08-24 deposited with the CCDC.	2020-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.23710(10)
_cell_length_b                   15.23710(10)
_cell_length_c                   155.7837(9)
_cell_measurement_reflns_used    13218
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.3410
_cell_measurement_theta_min      4.0730
_cell_volume                     31322.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (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      173
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.954
_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      4.00  29.05   0.15    1.37    --    5.00  41.00 156.00  167
  2  \w   -114.00  -6.00   0.15    1.37    --  -94.70  13.00  74.00  720
  3  \w    -73.00 -13.00   0.15    0.34    --    0.00  28.00-120.00  400
  4  \w     22.00  62.05   0.15    0.34    --    0.00  28.00-120.00  267
  5  \w   -166.00 -94.90   0.15    1.37    --  -94.70  46.00 120.00  474
  6  \w    -38.00 -11.90   0.15    1.37    --  -94.70  46.00 120.00  174
  7  \w    -56.00  -5.90   0.15    1.37    --  -94.70  18.00 150.00  334
  8  \w   -172.00 -65.95   0.15    1.37    --  -94.70  18.00 150.00  707
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0251700000
_diffrn_orient_matrix_UB_12      -0.0271072000
_diffrn_orient_matrix_UB_13      0.0095528000
_diffrn_orient_matrix_UB_21      0.0074160000
_diffrn_orient_matrix_UB_22      -0.0962860000
_diffrn_orient_matrix_UB_23      -0.0013135000
_diffrn_orient_matrix_UB_31      0.1137994000
_diffrn_orient_matrix_UB_32      0.0601947000
_diffrn_orient_matrix_UB_33      0.0021981000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.1088
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       153
_diffrn_reflns_limit_l_min       -192
_diffrn_reflns_number            32365
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.775
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    9.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       plate
_exptl_crystal_F_000             16668
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         13251
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+52.2882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10901
_reflns_number_total             13251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03386c2.cif
_cod_data_source_block           1_173K
_cod_original_cell_volume        31322.5(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7705859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONSNi
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.252
_diffrn_oxdiff_digest_frames
;
017dfcc6a7bd5a6a7f3031591f9fc8a9b7032438920
;
_diffrn_oxdiff_digest_hkl
;
01d500e6dfd2d58895b067da9b19d6cbde27c2
;
_reflns_odcompleteness_completeness 98.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-N9
 1.5 with sigma of 0.01
3. Rigid bond restraints
 N9, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C34 \\sim N16 \\sim C27 \\sim C28 \\sim N9 \\sim N10: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
N16 \\sim C34 \\sim C33 \\sim N15 \\sim N10 \\sim C28 \\sim C27 \\sim N9 \\sim
N7 \\sim C25 \\sim C26 \\sim N8: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N9 \\sim C27 \\sim C28 \\sim N10 \\sim N16 \\sim C34 \\sim C33: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C27, N9, C28, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, N16, C33, N15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C27, N9, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, N9, C28, N10, C33, C34, N16, N15, N7, C25, C26, N8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, C27, C28, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H12(0.16667) H11(0.16667) H13(0.16667) H46A(0.33333) H46B(0.33333)
 H46C(0.33333) H14(0.16667) H42A(0.33333) H42B(0.33333) H42C(0.33333)
 H44A(0.33333) H44B(0.33333) H44C(0.33333) H10(0.16667) H9(0.16667)
7.a Ternary CH refined with riding coordinates:
 N12(H12), N3(H3), N5(H5), N11(H11), N20(H20), N18(H18), N13(H13), N1(H1),
 N14(H14), N15(H15), N8(H8), N10(H10), N9(H9)
7.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C24(H24A,H24B), C36(H36A,H36B), C29(H29A,H29B), C21(H21A,
 H21B), C23(H23A,H23B), C37(H37A,H37B), C22(H22A,H22B), C35(H35A,H35B),
 C31(H31A,H31B), C38(H38A,H38B), C32(H32A,H32B), C19(H19A,H19B), C20(H20A,H20B),
  C26(H26A,H26B), C28(H28A,H28B), C25(H25A,H25B), C33(H33A,H33B), C34(H34A,
 H34B), C27(H27A,H27B)
7.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              34773
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.615