Carboxylic acid-tuned nickel(ii) clusters: syntheses, structures, solution behaviours and magnetic properties.
Su, Yan-Min; Ji, Bao-Qian; Shao, Feng; Zhang, Shan-Shan; Jagodič, Marko; Jagličić, Zvonko; Gao, Zhi-Yong; Dou, Jian-Min; Sun, Di; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4355–4362; doi:10.1039/d1dt00165e

data_7706689
_publ_section_title
;
 Carboxylic acid-tuned nickel(ii) clusters: syntheses, structures,
 solution behaviours and magnetic properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4355
_journal_page_last               4362
_journal_paper_doi               10.1039/d1dt00165e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C82 H94 N14 Ni6 O24, 4(C2 H3 N)'
_chemical_formula_sum            'C90 H106 N18 Ni6 O24'
_chemical_formula_weight         2176.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-01 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.6272(4)
_cell_length_b                   13.8653(2)
_cell_length_c                   23.2676(3)
_cell_measurement_reflns_used    13269
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3520
_cell_measurement_theta_min      3.9730
_cell_volume                     9966.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    -54.00  27.00   1.00    0.20    --  -48.32  19.00-150.00   81
  2  \w    -56.00 -13.00   1.00    0.80    --  -86.25  95.00-103.00   43
  3  \w    -79.00  17.00   1.00    0.20    --  -48.32  95.00-103.00   96
  4  \w    102.00 133.00   1.00    0.80    --  107.75  95.00-103.00   31
  5  \w     37.00 120.00   1.00    0.80    --  107.75 -37.00   0.00   83
  6  \w     35.00 121.00   1.00    0.80    --  107.75 -19.00 -30.00   86
  7  \w     36.00 118.00   1.00    0.80    --  107.75 -37.00 150.00   82
  8  \w     35.00 120.00   1.00    0.80    --  107.75 -57.00 150.00   85
  9  \w     44.00 103.00   1.00    0.80    --  107.75 -95.00 146.00   59
 10  \w   -143.00-118.00   1.00    0.80    --  -86.25 -95.00 146.00   25
 11  \w   -111.00 -71.00   1.00    0.20    --  -48.32-125.00 -60.00   40
 12  \w   -157.00-107.00   1.00    0.80    --  -86.25 -99.00 -90.00   50
 13  \w     53.00  78.00   1.00    0.20    --   48.32 -95.00 146.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0193929000
_diffrn_orient_matrix_UB_12      0.0962130000
_diffrn_orient_matrix_UB_13      0.0295927000
_diffrn_orient_matrix_UB_21      -0.0005053000
_diffrn_orient_matrix_UB_22      0.0384385000
_diffrn_orient_matrix_UB_23      -0.0623688000
_diffrn_orient_matrix_UB_31      -0.0459228000
_diffrn_orient_matrix_UB_32      0.0401378000
_diffrn_orient_matrix_UB_33      -0.0112133000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25662
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             4528
_exptl_crystal_recrystallization_method 173(K)
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+17.5482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7441
_reflns_number_total             8753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00165e2.cif
_cod_data_source_block           Ni6b
_cod_depositor_comments
'Adding full bibliography for 7706687--7706689.cif.'
_cod_database_code               7706689
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         NiCHON
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C17(H17), C34(H34), C12(H12), C10(H10), C18(H18), C11(H11),
 C6(H6), C3(H3A), C19(H19), C39(H39), C20(H20), C1(H1), C2(H2), C27(H27)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C7(H7A,H7B,H7C), C14(H14A,H14B,
 H14C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C22(H22A,H22B,H22C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.650