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_7709423
_publ_section_title
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 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 H40 B2 N6 Ni O6, C H2 Cl2'
_chemical_formula_sum            'C31 H42 B2 Cl2 N6 Ni O6'
_chemical_formula_weight         745.92
_chemical_name_systematic
(1,8-bisphenyl-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           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_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                108.029(2)
_cell_angle_beta                 91.507(2)
_cell_angle_gamma                100.848(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7045(3)
_cell_length_b                   12.6193(5)
_cell_length_c                   16.8514(6)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.61
_cell_volume                     1721.60(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.02
_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  0.0612
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49639
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.794
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.8787.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             713
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, ethyl ether'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.387(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         14029
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11983
_reflns_number_total             14029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02156g2.cif
_cod_data_source_block           jz113_0m_12102020_a
_cod_depositor_comments
'Adding full bibliography for 7709423--7709427.cif.'
_cod_database_code               7709423
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.851
_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.a Secondary CH2 refined with riding coordinates:
 C00R(H00A,H00B), C012(H01O,H01P), C014(H01Q,H01S), C01K(H01,H), C01T(H01H,
 H01I), C01V(H01J,H01K), C01X(H01L,H01M), C023(H02D,H02E), C024(H02Q,H02R),
 C02D(H02Z,HE), C02F(H02,HF), C02I(H02L,H02M), C02K(H6,HG), C02L(H7,HH)
2.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00Y(H00Y), C010(H010), C015(H015), C016(H016), C018(H018),
 C019(H019), C01A(H01D), C01C(H01X), C01J(H01Z), C01N(H01N), C01R(H01R),
 C01U(H01U), C01W(H3), C01Y(H01Y), C020(H020), C028(H028), C029(H029),
 C02C(H02Y), C02G(H4)
2.c Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C01B(H01T,H01V,H01W), C01M(H1,HA,HB), C01O(H01E,H01F,
 H01G), C01S(H2,HC,HD), C022(H02A,H02B,H02C), C025(H02S,H02T,H02U), C026(H02F,
 H02G,H02H), C02A(H02V,H02W,H02X), C02E(H02I,H02J,H02K), C02N(H02N,H02O,H02P),
 C02O(H5,HI,HJ)
;
_shelx_res_checksum              28783
_shelx_hkl_checksum              34860
_olex2_submission_special_instructions 'No special instructions were received'