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_7706687
_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         'C62 H70 N12 Ni4 O12, 2(N O3), 2(C2 H3 N)'
_chemical_formula_sum            'C66 H76 N16 Ni4 O18'
_chemical_formula_weight         1616.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-01
_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                 91.667(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7045(4)
_cell_length_b                   25.3661(6)
_cell_length_c                   17.6478(3)
_cell_measurement_reflns_used    15462
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.6360
_cell_measurement_theta_min      3.6590
_cell_volume                     7474.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_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     95.00 177.00   1.00    5.27    --  107.75  19.00 150.00   82
  2  \w    136.00 178.00   1.00    5.27    --  107.75  37.00  90.00   42
  3  \w    138.00 178.00   1.00    5.27    --  107.75  37.00 -30.00   40
  4  \w    109.00 135.00   1.00    5.27    --  107.75  37.00  90.00   26
  5  \w     85.00 111.00   1.00    5.27    --  107.75  77.00  -3.00   26
  6  \w     95.00 135.00   1.00    5.27    --  107.75  37.00 -30.00   40
  7  \w     76.00 131.00   1.00    5.27    --  107.75 -77.00-129.00   55
  8  \w     39.00 108.00   1.00    5.27    --  107.75 -99.00-150.00   69
  9  \w     38.00 103.00   1.00    5.27    --  107.75 -99.00-180.00   65
 10  \w      8.00  68.00   1.00    1.32    --   48.32 -77.00-129.00   60
 11  \w     41.00  71.00   1.00    1.32    --   48.32  77.00  -3.00   30
 12  \w    -71.00  24.00   1.00    1.32    --  -48.32  77.00  -3.00   95
 13  \w    -53.00 -27.00   1.00    5.27    --  -86.25  77.00  -3.00   26
 14  \w   -103.00 -26.00   1.00    1.32    --  -48.32 -77.00-129.00   77
 15  \w   -139.00 -63.00   1.00    5.27    --  -86.25 -77.00-129.00   76
 16  \w   -158.00 -83.00   1.00    5.27    --  -86.25 -99.00   0.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0022189000
_diffrn_orient_matrix_UB_12      -0.0200903000
_diffrn_orient_matrix_UB_13      -0.0823779000
_diffrn_orient_matrix_UB_21      -0.0539399000
_diffrn_orient_matrix_UB_22      0.0467966000
_diffrn_orient_matrix_UB_23      -0.0238051000
_diffrn_orient_matrix_UB_31      0.0748209000
_diffrn_orient_matrix_UB_32      0.0331232000
_diffrn_orient_matrix_UB_33      -0.0164208000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41900
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.592
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59011
_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    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         13102
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2700
_refine_ls_wR_factor_ref         0.2942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9896
_reflns_number_total             13102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00165e2.cif
_cod_data_source_block           Ni4a
_cod_depositor_comments
'Adding full bibliography for 7706687--7706689.cif.'
_cod_database_code               7706687
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         NiCHON
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.916
_reflns_odcompleteness_completeness 98.58
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-O16
 2.6 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 C59-H12
 1.909789 with sigma of 0.02
 Ni3-H12
 2.790437 with sigma of 0.02
 C60-H5
 1.893626 with sigma of 0.02
 Ni1-H5
 2.836745 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3A \\sim C2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C65 \\sim N13 \\sim C64: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
O16 \\sim O17 \\sim N16 \\sim O18: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
N16A \\sim O18A \\sim O17A \\sim O16A: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008
C3 \\sim C2 \\sim N1 \\sim N2 \\sim C4 \\sim C1: within 2A with sigma of 0.004
and sigma for terminal atoms of 0.008
N2A \\sim C4A \\sim C1A \\sim N1A \\sim C2A \\sim C3A: within 2A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(N16A) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(O17A) \\sim Ueq,
Uanis(O16A) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.2
4. Others
 Fixed Sof: N1(0.4) H1(0.4) N1A(0.6) H1A(0.6) C1(0.4) H1B(0.4) C1A(0.6)
 H1AA(0.6) C2(0.4) C2A(0.6) C3(0.4) H3A(0.4) H3B(0.4) H3C(0.4) C3A(0.6)
 H3AA(0.6) H3AB(0.6) H3AC(0.6) H5AA(0.4) H5AB(0.4) H5AC(0.4) H5BD(0.6)
 H5BE(0.6) H5BF(0.6) O16(0.5) O17(0.5) O18(0.5) N16(0.5) O18A(0.5) O17A(0.5)
 O16A(0.5) N16A(0.5) C4(0.4) N2(0.4) N2A(0.6) C4A(0.6)
5.a Ternary CH refined with riding coordinates:
 C58(H58), C59(H59), C60(H60), C61(H61)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N1A(H1A), N12(H12A), C1(H1B), C1A(H1AA), C8(H8), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C40(H40), C45(H45), C50(H50), C55(H55)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C5(H5AA,H5AB,H5AC), C5(H5BD,H5BE,H5BF),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C),
  C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C64(H64A,H64B,H64C), C63(H63A,
 H63B,H63C)
;
_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 4.989
_oxdiff_exptl_absorpt_empirical_full_min 0.473