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_7706992
_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, 2(C H4 O)'
_chemical_formula_sum            'C42 H74 Cl2 N4 Ni4 O16'
_chemical_formula_weight         1196.79
_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   geom
_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                 109.740(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9472(8)
_cell_length_b                   24.8080(6)
_cell_length_c                   10.1468(3)
_cell_measurement_reflns_used    9089
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.1
_cell_measurement_theta_min      1.8
_cell_volume                     2593.7(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      100
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28828
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         3.563
_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    3.154
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0652P)^2^+13.6462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3856
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04286b2.cif
_cod_data_source_block           ssw420_p21c
_cod_depositor_comments
'Adding full bibliography for 7706989--7706992.cif.'
_cod_original_cell_volume        2593.7(2)
_cod_database_code               7706992
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.557
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C51(H51)
3.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C53(H53A,H53B)
3.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C34(H34), C38(H38)
3.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C60(H60A,H60B,H60C), C67(H67A,H67B,
 H67C), C69(H69A,H69B,H69C), C73(H73A,H73B,H73C), C77(H77A,H77B,H77C), C80(H80A,
 H80B,H80C), C1(H1A,H1B,H1C)
3.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O8(H8)
;
_shelx_res_checksum              77796
_olex2_submission_special_instructions 'No special instructions were received'