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_7709425
_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         'C34 H48 B2 N6 Ni O10'
_chemical_formula_sum            'C34 H48 B2 N6 Ni O10'
_chemical_formula_weight         781.09
_chemical_name_common            Ni-Et-OMe
_chemical_name_systematic
(1,8-bis(3,5-dimethoxyphenyl)-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      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-10-20 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.800(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8983(12)
_cell_length_b                   8.7226(4)
_cell_length_c                   17.7343(7)
_cell_measurement_reflns_used    8197
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.35
_cell_volume                     3680.6(3)
_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      100.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1308
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45374
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         2.985
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0898 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.8193.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       Diamond
_exptl_crystal_F_000             1648.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane'
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3137
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0354P)^2^+37.8187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2532
_reflns_number_total             3142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02156g2.cif
_cod_data_source_block           jz109_0m_02172021_a
_cod_depositor_comments
'Adding full bibliography for 7709423--7709427.cif.'
_cod_database_code               7709425
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.858
_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. Restrained distances
 C00R-C00P = C00P-C00C
 1.5 with sigma of 0.02
 C00P-C00C = C00R-C00P
 1.5 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00O(H00O,H00P), C00P(H00Q,H00R)
3.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00G(H00G)
3.c Idealised Me refined as rotating group:
 C00J(H00C,H00F,H00H), C00K(H00I,H00J,H00K), C00M(H00L,H00M,H00N), C00Q(H00S,
 H00T,H00U), C00R(H00V,H00W,H00X)
;
_shelx_res_checksum              45912
_shelx_hkl_checksum              78986
_olex2_submission_special_instructions 'No special instructions were received'