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_7706989
_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         'C40 H66 Cl2 N4 Ni4 O14, 3(C4 H10 O)'
_chemical_formula_sum            'C52 H96 Cl2 N4 Ni4 O17'
_chemical_formula_weight         1355.06
_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     iterative
_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                 90.34
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3361(6)
_cell_length_b                   13.8643(7)
_cell_length_c                   17.3381(12)
_cell_measurement_reflns_used    3770
_cell_measurement_temperature    123
_cell_measurement_theta_max      69.9
_cell_measurement_theta_min      2.5
_cell_volume                     3205.7(3)
_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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45885
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         6.021
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.79
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1049P)^2^+5.1910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5563
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04286b2.cif
_cod_data_source_block           ssw383
_cod_depositor_comments
'Adding full bibliography for 7706989--7706992.cif.'
_cod_database_code               7706989
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.496
_shelx_estimated_absorpt_t_min   0.231
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C1AA) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(C3AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Rigid body (RIGU) restrains
 C0AA, O9, C1AA, C2AA, C3AA
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Others
 Fixed Sof: O9(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C1AA(0.5)
 H1AA(0.5) H1AB(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) C3AA(0.5) H3AA(0.5)
 H3AB(0.5) H3AC(0.5)
5.a Free rotating group:
 O9(C0AA,C1AA,C2AA,C3AA)
5.b Ternary CH refined with riding coordinates:
 C65(H65)
5.c Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C61(H61A,H61B), C00T(H00G,H00H), C00U(H00I,H00J), C1AA(H1AA,
 H1AB), C2AA(H2AA,H2AB)
5.d Aromatic/amide H refined with riding coordinates:
 C21(H21), C5(H5A), C3(H3)
5.e Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C), C31(H31A,H31B,H31C), C63(H63A,H63B,H63C), C69(H69A,H69B,
 H69C), C00W(H00D,H00E,H00F), C00X(H00K,H00L,H00M), C67(H67A,H67B,H67C),
 C00Z(H00N,H00O,H00P), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C0AA(H0AA,
 H0AB,H0AC), C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              59147
_olex2_submission_special_instructions 'No special instructions were received'