The structural manipulation of a series of Ni<sub>4</sub> defective dicubanes: Synthesis, X-ray Structures, Magnetic and Computational analyses.
Woodhouse, Sidney S.; Dais, Tyson N.; Payne, Emily H.; Singh, Mukesh K.; Brechin, Euan K.; Plieger, Paul G.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5318–5326; doi:10.1039/d0dt04286b

data_7706991
_publ_section_title
;
 The structural manipulation of a series of Ni<sub>4</sub> defective
 dicubanes: Synthesis, X-ray Structures, Magnetic and Computational
 analyses.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5318
_journal_page_last               5326
_journal_paper_doi               10.1039/d0dt04286b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C38 H68 Cl4 N4 Ni4 O12, C4 H10 O'
_chemical_formula_sum            'C42 H78 Cl4 N4 Ni4 O13'
_chemical_formula_weight         1223.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-25 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.181(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1613(11)
_cell_length_b                   20.497(2)
_cell_length_c                   25.796(3)
_cell_measurement_reflns_used    1098
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.5
_cell_measurement_theta_min      3.4
_cell_volume                     5371.6(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.2394
_diffrn_reflns_av_unetI/netI     0.4683
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42778
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         70.079
_diffrn_reflns_theta_min         2.754
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_target            Mo
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2568
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         9809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.2708
_refine_ls_R_factor_gt           0.0941
_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^)+(0.0891P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2911
_reflns_number_total             9809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04286b2.cif
_cod_data_source_block           ssw410i
_cod_depositor_comments
'Adding full bibliography for 7706989--7706992.cif.'
_cod_original_cell_volume        5371.6(11)
_cod_database_code               7706991
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.387
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C00X(H00X), C017(H017)
2.b Secondary CH2 refined with riding coordinates:
 C014(H01D,H01E), C019(H01L,H01M), C01E(H01T,H01U), C01G(H12,H), C01I(H01Z,HA),
  C01N(H13,HJ)
2.c Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00U(H00U), C00W(H00W), C012(H012), C015(H015), C01H(H01Y)
2.d Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C016(H01F,H01G,H01H), C018(H01I,H01J,H01K), C01A(H01N,
 H01O,H01P), C01D(H01Q,H01R,H01S), C01F(H01V,H01W,H01X), C01J(H01,HB,HC),
 C01K(H1,HD,HE), C01L(H2,HF,HG), C01M(H3,HH,HI), C01O(H4,HK,HL), C01P(H7,HM,HN),
  C01Q(H14,HO,HP), C01R(H8,HQ,HR), C01S(H9,HS,HT), C01T(H10,HU,HV), C01U(H11,HW,
 HX), C01V(H15,HY,HZ)
2.e Idealised tetrahedral OH refined as rotating group:
 O00I(H00I)
;
_shelx_res_checksum              15510
_olex2_submission_special_instructions 'No special instructions were received'