Anionic oxoborane and thioxoborane molecules supported by a 1,2-bis(imino)acenaphthene ligand.
Liu, Rui; Gao, Fangfang; Liu, Jingjing; Wei, Jing; Hou, Lei; Xie, Gang; Chen, Sanping; Zeng, Fanlong; Li, Anyang; Wang, Wenyuan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6797–6801; doi:10.1039/d1dt01060c

data_7707297
_publ_section_title
;
 Anionic oxoborane and thioxoborane molecules supported by a
 1,2-bis(imino)acenaphthene ligand.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6797
_journal_page_last               6801
_journal_paper_doi               10.1039/d1dt01060c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '3(C36 H40 B N2 O), 3(C11 H21 N2), 2(C7 H8)'
_chemical_formula_sum            'C155 H199 B3 N12 O3'
_chemical_formula_weight         2310.68
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-15 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                82.716(3)
_cell_angle_beta                 68.186(3)
_cell_angle_gamma                60.437(3)
_cell_formula_units_Z            2
_cell_length_a                   19.0151(12)
_cell_length_b                   19.0592(13)
_cell_length_c                   24.0200(16)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      68.01
_cell_measurement_theta_min      3.44
_cell_volume                     7012.4(8)
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_collection       'Bruker D8 Quest'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            124361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.309
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    0.490
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1693
_refine_ls_number_reflns         25511
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+1.8487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19929
_reflns_number_total             25511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01060c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707295--7707297.cif.'
_cod_database_code               7707297
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C161-C160 = C84-C88 = C84-C87 = C84-C85 = C84-C86
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C31, C33
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.006
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C92 \\sim C94: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C160) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C150)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C148)=Sof(H14P)=Sof(H14Q)=
 Sof(H14R)=Sof(C152)=Sof(H15G)=Sof(H15H)=Sof(H15I)=1-FVAR(1)
 Sof(C147)=Sof(H14J)=Sof(H14K)=Sof(H14L)=Sof(C149)=Sof(H14M)=Sof(H14N)=
 Sof(H14O)=Sof(C151)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C100)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C102)=Sof(H10G)=Sof(H10H)=Sof(H10I)=1-FVAR(2)
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=
 Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(H84A)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(H88C)=1-FVAR(3)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=
 Sof(H84)=FVAR(3)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(4)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(4)
6.a Riding coordinates:
 C33(H33A,H33B,H33C), C87(H84), C85(H84A)
6.b Ternary CH refined with riding coordinates:
 C19(H19), C23(H23), C31(H31), C34(H34), C69(H69), C72(H72), C81(H81),
 C121(H121), C124(H124), C133(H133), C136(H136)
6.c Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C), C85(H85A,H85B,H85C), C88(H88A,H88B,H88C), C97(H97A,H97B,H97C),
 C99(H99A,H99B,H99C), C101(H10A,H10B,H10C), C98(H98A,H98B,H98C), C100(H10D,H10E,
 H10F), C102(H10G,H10H,H10I), C147(H14J,H14K,H14L), C149(H14M,H14N,H14O),
 C151(H15A,H15B,H15C), C150(H15D,H15E,H15F), C148(H14P,H14Q,H14R), C152(H15G,
 H15H,H15I)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C27(H27), C28(H28), C29(H29), C37(H37), C38(H38), C39(H39), C54(H54),
  C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C65(H65), C66(H66),
 C67(H67), C77(H77), C78(H78), C79(H79), C89(H89), C90(H90), C91(H91),
 C106(H106), C107(H107), C108(H108), C110(H110), C111(H111), C112(H112),
 C117(H117), C118(H118), C119(H119), C129(H129), C130(H130), C131(H131),
 C139(H139), C140(H140), C141(H141), C155(H155), C156(H156), C157(H157),
 C158(H158), C159(H159), C162(H162), C163(H163), C164(H164), C165(H165),
 C166(H166)
6.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,
 H95B,H95C), C122(H12A,H12B,H12C), C123(H12D,H12E,H12F), C125(H12G,H12H,H12I),
 C126(H12J,H12K,H12L), C134(H13A,H13B,H13C), C135(H13D,H13E,H13F), C137(H13G,
 H13H,H13I), C138(H13J,H13K,H13L), C143(H14A,H14B,H14C), C144(H14D,H14E,H14F),
 C145(H14G,H14H,H14I), C153(H15J,H15K,H15L), C160(H16A,H16B,H16C)
;
_shelx_res_checksum              63912
_shelx_hkl_checksum              44024
_olex2_submission_special_instructions 'No special instructions were received'