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_7705861
_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             2020-07-09
_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                   15.28410(10)
_cell_length_b                   15.28410(10)
_cell_length_c                   155.7874(9)
_cell_measurement_reflns_used    34615
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.4440
_cell_measurement_theta_min      2.5810
_cell_volume                     31516.8(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      223
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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    -86.00 -41.90   0.15    0.37    --    0.00  55.00   0.00  294
  2  \w    -44.00  75.10   0.15    0.37    --    0.00  46.00 150.00  794
  3  \w    -81.00 -54.00   0.15    0.37    --    0.00  46.00 150.00  180
  4  \w   -115.00 -82.00   0.15    1.47    --  -94.70  46.00-180.00  220
  5  \w    -91.00 -64.00   0.15    1.47    --  -94.70   0.00-150.00  180
  6  \w   -184.00-154.00   0.15    1.47    --  -94.70  37.00   0.00  200
  7  \w   -113.00  -5.00   0.15    1.47    --  -94.70  18.00-180.00  720
  8  \w   -182.00-128.00   0.15    1.47    --  -94.70  18.00-180.00  360
  9  \w   -149.00  -9.95   0.15    1.47    --  -94.70  37.00   0.00  927
 10  \w   -184.00-124.90   0.15    1.47    --  -94.70   0.00-150.00  394
 11  \w    -47.00  -5.90   0.15    1.47    --  -94.70  46.00-180.00  274
 12  \w    -65.00 -40.85   0.15    1.47    --  -94.70  28.00 150.00  161
 13  \w    -36.00  -9.90   0.15    1.47    --  -94.70  28.00 150.00  174
 14  \w   -173.00-148.85   0.15    1.47    --  -94.70  46.00-180.00  161
 15  \w    -71.00 -33.05   0.15    1.47    --  -94.70   0.00-120.00  253
 16  \w   -181.00  -5.95   0.15    1.47    --  -94.70  37.00  30.00 1167
;
_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      -0.0025562000
_diffrn_orient_matrix_UB_12      -0.1020407000
_diffrn_orient_matrix_UB_13      -0.0001209000
_diffrn_orient_matrix_UB_21      -0.0301031000
_diffrn_orient_matrix_UB_22      -0.0156589000
_diffrn_orient_matrix_UB_23      0.0095524000
_diffrn_orient_matrix_UB_31      -0.1123990000
_diffrn_orient_matrix_UB_32      -0.0537390000
_diffrn_orient_matrix_UB_33      -0.0025564000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       188
_diffrn_reflns_limit_l_min       -190
_diffrn_reflns_number            74900
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.848
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    9.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44869
_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    1.720
_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         0.727
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         13824
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+47.9327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12117
_reflns_number_total             13824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03386c2.cif
_cod_data_source_block           1_223K
_cod_original_cell_volume        31516.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7705861
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N OSNi'
_shelx_estimated_absorpt_t_max   0.573
_shelx_estimated_absorpt_t_min   0.254
_diffrn_oxdiff_digest_frames
;
01e646be389c07ffc9572f06043232c87d064598ea3
;
_diffrn_oxdiff_digest_hkl
;
018edb8cc00981a54a7c6bace09cef8b5e0f32
;
_reflns_odcompleteness_completeness 99.98
_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
 C33-N15
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: H18(0.16667) H17(0.16667) H19(0.16667) H42A(0.33333) H42B(0.33333)
 H42C(0.33333) H20(0.16667) H44A(0.33333) H44B(0.33333) H44C(0.33333)
 H40A(0.33333) H40B(0.33333) H40C(0.33333) H16(0.16667) H15(0.16667)
5.a Ternary CH refined with riding coordinates:
 N18(H18), N12(H12), N17(H17), N14(H14), N4(H4), N6(H6), N19(H19), N8(H8),
 N20(H20), N9(H9), N1(H1), N16(H16), N15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C36(H36A,H36B), C29(H29A,H29B), C23(H23A,H23B), C35(H35A,
 H35B), C22(H22A,H22B), C24(H24A,H24B), C31(H31A,H31B), C21(H21A,H21B),
 C37(H37A,H37B), C32(H32A,H32B), C38(H38A,H38B), C25(H25A,H25B), C26(H26A,H26B),
  C19(H19A,H19B), C20(H20A,H20B), C34(H34A,H34B), C27(H27A,H27B), C28(H28A,
 H28B), C33(H33A,H33B)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              44991
_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 1.975
_oxdiff_exptl_absorpt_empirical_full_min 0.759