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_7705860
_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                   15.1802(2)
_cell_length_b                   15.1802(2)
_cell_length_c                   155.6425(13)
_cell_measurement_reflns_used    22401
_cell_measurement_temperature    123
_cell_measurement_theta_max      72.5480
_cell_measurement_theta_min      3.3510
_cell_volume                     31060.9(6)
_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      123
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -24.00   1.00   0.50    6.62    --    0.00  27.00 -46.00   50
  2  \w    -19.00   6.00   0.50   26.46    --    5.00  27.00 -46.00   50
  3  \w    -99.00 -47.00   0.50   26.46    --  -94.70  27.00 -46.00  104
  4  \w    -87.00 -62.00   0.50    6.62    --    0.00  28.00-150.00   50
  5  \w     44.00  85.00   0.50    6.62    --    0.00  28.00-150.00   82
  6  \w    -89.00  50.00   0.50    6.62    --    0.00   9.00  30.00  278
  7  \w   -100.00 -74.00   0.50   26.46    --  -94.70  37.00  90.00   52
  8  \w   -129.00-103.00   0.50   26.46    --  -94.70  18.00 -90.00   52
  9  \w   -184.00  -6.00   0.50   26.46    --  -94.70  46.00 150.00  356
 10  \w   -181.00-156.00   0.50   26.46    --  -94.70  18.00 -90.00   50
 11  \w    -88.00 -46.00   0.50   26.46    --  -94.70   9.00 -60.00   84
 12  \w   -101.00 -75.00   0.50   26.46    --  -94.70   9.00-150.00   52
 13  \w    -54.00 -28.00   0.50   26.46    --  -94.70   9.00-150.00   52
 14  \w   -143.00  -5.00   0.50   26.46    --  -94.70  46.00-150.00  276
 15  \w   -184.00-119.00   0.50   26.46    --  -94.70  46.00  90.00  130
 16  \w   -111.00 -12.00   0.50   26.46    --  -94.70  46.00  90.00  198
 17  \w   -165.00 -97.00   0.50   26.46    --  -94.70   9.00 -60.00  136
 18  \w   -146.00-121.00   0.50   26.46    --  -94.70  37.00  90.00   50
 19  \w   -182.00-157.00   0.50   26.46    --  -94.70  37.00  90.00   50
;
_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      0.0211427000
_diffrn_orient_matrix_UB_12      0.0476780000
_diffrn_orient_matrix_UB_13      0.0090397000
_diffrn_orient_matrix_UB_21      0.0862967000
_diffrn_orient_matrix_UB_22      -0.0243493000
_diffrn_orient_matrix_UB_23      0.0012000000
_diffrn_orient_matrix_UB_31      0.0763789000
_diffrn_orient_matrix_UB_32      0.1042467000
_diffrn_orient_matrix_UB_33      -0.0038567000
_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  0.0856
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       138
_diffrn_reflns_limit_l_min       -192
_diffrn_reflns_number            68632
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.969
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    9.776
_exptl_absorpt_correction_T_max  0.08938
_exptl_absorpt_correction_T_min  0.01342
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.745
_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
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.145
_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         13667
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1087P)^2^+45.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12370
_reflns_number_total             13667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03386c2.cif
_cod_data_source_block           1_123K
_cod_original_cell_volume        31060.9(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7705860
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N OSNi'
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.250
_diffrn_oxdiff_digest_frames
;
01f0659071ef7eb96102548ee956c74a4d02152a8f7
;
_diffrn_oxdiff_digest_hkl
;
011294dd896130dd37a6ac3dddcd401028b88a
;
_reflns_odcompleteness_completeness 99.96
_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
 N19-N20
 2.54 with sigma of 0.02
 C32-N14 = C31-N13
 1.5 with sigma of 0.02
 C31-C32
 1.54 with sigma of 0.02
 N7-C25_$1 = N8-C26_$1
 1.5 with sigma of 0.02
 N7-N8 = N13_$3-N14_$3
 2.54 with sigma of 0.02
 N9-C27
 1.5 with sigma of 0.02
 N19-C45_$2
 1.468 with sigma of 0.02
 N19-C46_$2
 2.469 with sigma of 0.04
 C45-N20
 2.469 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N19 \\sim C45 \\sim C46 \\sim N10 \\sim C28 \\sim N9 \\sim C27: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H11(0.16667) H12(0.16667) H10(0.16667) H9(0.16667) H40A(0.33333)
 H40B(0.33333) H40C(0.33333) H42A(0.33333) H42B(0.33333) H42C(0.33333)
 H43A(0.33333) H43B(0.33333) H43C(0.33333) H13(0.16667) H14(0.16667)
6.a Ternary CH refined with riding coordinates:
 N3(H3), N11(H11), N5(H5), N12(H12), N15(H15), N17(H17), N1(H1), N10(H10),
 N9(H9), N20(H20), N8(H8), N13(H13), N14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C24(H24A,H24B), C23(H23A,H23B), C21(H21A,H21B), C35(H35A,
 H35B), C22(H22A,H22B), C36(H36A,H36B), C30(H30A,H30B), C34(H34A,H34B),
 C28(H28A,H28B), C20(H20A,H20B), C19(H19A,H19B), C33(H33A,H33B), C27(H27A,H27B),
  C46(H46A,H46B), C26(H26A,H26B), C45(H45A,H45B), C25(H25A,H25B), C31(H31A,
 H31B), C32(H32A,H32B)
6.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              73398
_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 1.976
_oxdiff_exptl_absorpt_empirical_full_min 0.582