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_7706990
_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 Cl2.8 F1.2 N4 Ni4 O12, C4 H10 O'
_chemical_formula_sum            'C42 H78 Cl2.8 F1.2 N4 Ni4 O13'
_chemical_formula_weight         1203.98
_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
_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                 90.155(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5697(8)
_cell_length_b                   21.0552(14)
_cell_length_c                   26.071(2)
_cell_measurement_reflns_used    5690
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.8
_cell_measurement_theta_min      2.1
_cell_volume                     5253.1(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.1568
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38116
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         66.000
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_target            Mo
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.471
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             2530
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         9133
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0967P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5545
_reflns_number_total             9133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04286b2.cif
_cod_data_source_block           ssw416i
_cod_depositor_comments
'Adding full bibliography for 7706989--7706992.cif.'
_cod_original_formula_sum        'C42 H78 Cl2.80 F1.20 N4 Ni4 O13'
_cod_database_code               7706990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.642
_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. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 C01P-H5
 1.948338 with sigma of 0.02
 Ni1-H5
 2.668334 with sigma of 0.02
3. Others
 Fixed Sof: Cl2(0.4) Cl1(0.4) F2(0.6) F1(0.6)
 Fixed X: H00I(0.50504) H00K(-0.034591)
 Fixed Y: H00I(0.41842) H00K(0.375509)
 Fixed Z: H00I(0.14691) H00K(0.346469)
4.a Ternary CH refined with riding coordinates:
 C015(H015), C01G(H01Z)
4.b Secondary CH2 refined with riding coordinates:
 C011(H01A,H01B), C017(H01F,H01G), C01H(H01,HA), C01I(H1,HB), C01K(H13,HE),
 C01R(H16,HR)
4.c Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C01C(H01Q)
4.d Idealised Me refined as rotating group:
 C016(H01C,H01D,H01E), C018(H01H,H01I,H01J), C019(H01K,H01L,H01M), C01B(H01N,
 H01O,H01P), C01D(H01R,H01S,H01T), C01E(H01U,H01V,H01W), C01F(H01X,H01Y,H),
 C01J(H2,HC,HD), C01L(H3,HF,HG), C01M(H4,HH,HI), C01N(H14,HJ,HK), C01O(H7,HL,
 HM), C01P(H8,HN,HO), C01Q(H15,HP,HQ), C01S(H9,HS,HT), C01T(H10,HU,HV),
 C01U(H11,HW,HX), C01V(H12,HY,HZ)
4.e Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              28688
_olex2_submission_special_instructions 'No special instructions were received'