Development of electronically tuneable N-heterocyclic borates.
Huerfano, I. J.; Gorobets, Evgueni; Zhou, Wen; Piers, Warren E.; Van Humbeck, Jeffrey F.; Derksen, Darren J.; Chemical communications (Cambridge, England) 61 (2025) 10610–10613; doi:10.1039/d5cc01578b

data_7134733
_publ_section_title
;
 Development of electronically tuneable N-heterocyclic borates.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10610
_journal_page_last               10613
_journal_paper_doi               10.1039/d5cc01578b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'6(C32 H44 B Mg0.5 N8), 6(C4 H8 O), 6(C0.458 H1)'
_chemical_formula_sum            'C218.75 H318 B6 Mg3 N48 O6'
_chemical_formula_weight         3853.98
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   41.4755(4)
_cell_length_b                   41.4755(4)
_cell_length_c                   11.7891(2)
_cell_measurement_reflns_used    8850
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      72.59
_cell_measurement_theta_min      3.69
_cell_volume                     17562.8(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32293
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.581
_diffrn_reflns_theta_min         3.692
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0752 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.9206.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       Block
_exptl_crystal_F_000             6242
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7620
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1854P)^2^+9.7522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5648
_reflns_number_total             7620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01578b2.cif
_cod_data_source_block           mg[b(pm)4]2_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134731--7134734.cif.
;
_cod_original_cell_volume        17562.8(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7134733
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.893
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 C54-C53 = C53-C52 = C52-C51 = C51-C50
 1.54 with sigma of 0.01
 C53-C51 = C50-C52 = C52-C54
 2.2 with sigma of 0.01
 C36-C54 = C54-C50
 3.825 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C34 \\sim C40 \\sim C39 \\sim C45 \\sim C46 \\sim C47: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C34) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.002
4. Others
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: Mg1(0.5) C50(0.041667) H50A(0.020833) H50B(0.020833)
 H50C(0.020833) H50D(0.020833) H50E(0.020833) H50F(0.020833) C51(0.125)
 H51A(0.125) H51B(0.125) C52(0.125) H52A(0.125) H52B(0.125) C53(0.125)
 H53A(0.125) H53B(0.125) C54(0.041667) H54A(0.020833) H54B(0.020833)
 H54C(0.020833) H54D(0.020833) H54E(0.020833) H54F(0.020833)
5.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C51(H51A,
 H51B), C52(H52A,H52B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C8(H8), C12(H12), C16(H16), C20(H20), C22(H22), C26(H26)
5.c Disordered Me refined with riding coordinates:
 C50(H50A,H50B,H50C,H50D,H50E,H50F), C54(H54A,H54B,H54C,H54D,H54E,H54F)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C)
;
_shelx_res_checksum              46079
_shelx_hkl_checksum              28906
_olex2_submission_special_instructions 'No special instructions were received'