Ligand design of zero-field splitting in trigonal prismatic Ni(II) cage complexes.
Campanella, Anthony J.; Ozvat, Tyler M.; Zadrozny, Joseph M.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 3341–3348; doi:10.1039/d1dt02156g

data_7709427
_publ_section_title
;
 Ligand design of zero-field splitting in trigonal prismatic Ni(II) cage
 complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3341
_journal_page_last               3348
_journal_paper_doi               10.1039/d1dt02156g
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C30 H30 B2 F10 N6 Ni O6'
_chemical_formula_sum            'C30 H30 B2 F10 N6 Ni O6'
_chemical_formula_weight         840.91
_chemical_name_systematic
(1,8-bis(pentafluorophenyl)-4,5,11,12,17,18-hexaethyl-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza-1,8-diboratabicyclo[6.6.6]icosa-3,5,10,12,16,18-hexaene)-nickel
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-05-26 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                67.6230(10)
_cell_angle_beta                 88.3260(10)
_cell_angle_gamma                71.7290(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7082(3)
_cell_length_b                   12.2248(3)
_cell_length_c                   13.9254(4)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    104.13
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      2.31
_cell_volume                     1740.90(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      104.13
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            96810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.590
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.8769.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, Ethyl ether'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0635P)^2^+2.0365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6043
_reflns_number_total             7132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02156g2.cif
_cod_data_source_block           jz111_0m_11162020_a
_cod_depositor_comments
'Adding full bibliography for 7709423--7709427.cif.'
_cod_database_code               7709427
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C01G(0.5) H01N(0.5) H01O(0.5) C01J(0.67) H01V(0.67) H01W(0.67)
 H01X(0.67) C01K(0.33) H01Y(0.33) H(0.33) HA(0.33) C1(0.5) H1A(0.5) H1B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C00T(H00A,H00B), C00X(H00C,H00D), C00Z(H00E,H00F), C018(H01A,H01B), C01A(H01F,
 H01G), C01G(H01N,H01O), C1(H1A,H1B)
3.b Idealised Me refined as rotating group:
 C019(H01C,H01D,H01E), C01B(H01H,H01I,H01J), C01F(H01K,H01L,H01M), C01H(H01P,
 H01Q,H01R), C01I(H01S,H01T,H01U), C01J(H01V,H01W,H01X), C01K(H01Y,H,HA)
;
_shelx_res_checksum              49157
_shelx_hkl_checksum              4636
_olex2_submission_special_instructions 'No special instructions were received'