Self-assembly of a nonanuclear Ni<sup>II</sup> cluster via atmospheric CO<sub>2</sub> fixation: synthesis, structure, collision-induced dissociation mass spectrometry and magnetic property.
Tian, Xue-Fei; Ji, Bao-Qian; Feng, Lei; Sheng, Kai; Su, Yan-Min; Jagodič, Marko; Jagličić, Zvonko; Tung, Chen-Ho; Sun, Di; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10977–10982; doi:10.1039/d0dt01573c

data_7704839
_publ_section_title
;
 Self-assembly of a nonanuclear Ni<sup>II</sup> cluster via atmospheric
 CO<sub>2</sub> fixation: synthesis, structure, collision-induced
 dissociation mass spectrometry and magnetic property.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10977
_journal_page_last               10982
_journal_paper_doi               10.1039/d0dt01573c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C94 H108 N14 Ni9 O30, 2(C3 H7 N O), C2 H6 O'
_chemical_formula_sum            'C102 H128 N16 Ni9 O33'
_chemical_formula_weight         2634.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2020-03-29 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                103.9220(10)
_cell_angle_beta                 90.0550(10)
_cell_angle_gamma                112.649(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8190(3)
_cell_length_b                   15.4014(3)
_cell_length_c                   28.1536(3)
_cell_measurement_reflns_used    32900
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2580
_cell_measurement_theta_min      3.1510
_cell_volume                     5724.3(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.981
_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   -120.00 -83.00   1.00    0.12    --  -48.45 -51.00  58.00   37
  2  \w    -22.00  62.00   1.00    0.12    --   48.45 -51.00  58.00   84
  3  \w     38.00 119.00   1.00    0.12    --   48.45  51.00-155.00   81
  4  \w   -100.00 -58.00   1.00    0.60    --  -86.25  51.00-155.00   42
  5  \w   -155.00 -72.00   1.00    0.60    --  -86.25 -51.00  58.00   83
  6  \w    -52.00 -14.00   1.00    0.60    --  -86.25  51.00-155.00   38
  7  \w     93.00 152.00   1.00    0.60    --  106.49  51.00-155.00   59
  8  \w     35.00 120.00   1.00    0.60    --  106.49 -51.00  58.00   85
  9  \w    -80.00 -36.00   1.00    0.12    --  -48.45 -51.00  58.00   44
 10  \w    -60.00 -25.00   1.00    0.12    --  -48.45  51.00-155.00   35
 11  \w   -123.00 -40.00   1.00    0.12    --  -48.45 -19.00 -60.00   83
 12  \w    -24.00  21.00   1.00    0.12    --  -48.45  51.00-155.00   45
 13  \w    102.00 178.00   1.00    0.60    --  106.49  19.00  90.00   76
 14  \w     32.00 119.00   1.00    0.60    --  106.49 -19.00-150.00   87
 15  \w     34.00 109.00   1.00    0.60    --  106.49 -99.00  30.00   75
 16  \w     89.00 122.00   1.00    0.60    --  106.49  77.00 -60.00   33
 17  \w     94.00 168.00   1.00    0.60    --  106.49 125.00 120.00   74
 18  \w    127.00 177.00   1.00    0.60    --  106.49  77.00 -60.00   50
 19  \w     34.00 128.00   1.00    0.60    --  106.49 -77.00  30.00   94
 20  \w     38.00 107.00   1.00    0.60    --  106.49 -99.00 -60.00   69
 21  \w     93.00 177.00   1.00    0.60    --  106.49 125.00   0.00   84
 22  \w     38.00 117.00   1.00    0.60    --  106.49-125.00 -60.00   79
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0829317000
_diffrn_orient_matrix_UB_12      0.0189076000
_diffrn_orient_matrix_UB_13      -0.0228518000
_diffrn_orient_matrix_UB_21      0.0509746000
_diffrn_orient_matrix_UB_22      0.1091786000
_diffrn_orient_matrix_UB_23      0.0265874000
_diffrn_orient_matrix_UB_31      0.0579065000
_diffrn_orient_matrix_UB_32      0.0181568000
_diffrn_orient_matrix_UB_33      -0.0445449000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            56053
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1477
_refine_ls_number_reflns         20035
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0738P)^2^+11.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16741
_reflns_number_total             20035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01573c2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 7704839.cif.'
_cod_original_cell_volume        5724.34(19)
_cod_database_code               7704839
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         NiC
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.876
_reflns_odcompleteness_completeness 98.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, H6 of O6, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, HG of O32
2. Restrained distances
 H11-O11
 0.89 with sigma of 0.01
 C91-C94
 1.55 with sigma of 0.01
 O32-C91
 1.35 with sigma of 0.01
3.a Riding coordinates:
 O32(HG)
3.b Ternary CH refined with riding coordinates:
 O3(H3), O6(H6)
3.c Secondary CH2 refined with riding coordinates:
 C91(HH,HI)
3.d Me refined with riding coordinates:
 C97(H97A,H97B,H97C)
3.e Aromatic/amide H refined with riding coordinates:
 N3(H3A), N6(H6A), N9(H9), N10(H10), N11(H11A), N12(H12), C2AA(H2AA), C9(H9A),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C37(H37), C38(H38),
  C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C47(H47), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67),
 C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C83(H83), C84(H84), C85(H85), C88(H88),
 C89(H89), C82(H), C95(HM)
3.f Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C41(H41A,H41B,H41C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C54(H54A,H54B,H54C), C63(H63A,
 H63B,H63C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C92(H92A,H92B,H92C), C96(H96A,H96B,H96C), C99(H99A,H99B,
 H99C), C90(HA,HB,HC), C93(HD,HE,HF), C94(HJ,HK,HL), C98(HN,HO,HP), C100(HQ,HR,
 HS)
;
_shelx_res_checksum              25694
_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.658