CAAC-stabilised 9,10-diboraanthracene: an electronically and structurally flexible platform for small-molecule activation and metal complexation.
Dietz, Maximilian; Arrowsmith, Merle; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003) 53 (2024) 449–453; doi:10.1039/d3dt03787h

data_7714664
_publ_section_title
;
 CAAC-stabilised 9,10-diboraanthracene: an electronically and structurally
 flexible platform for small-molecule activation and metal complexation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              449
_journal_page_last               453
_journal_paper_doi               10.1039/d3dt03787h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C55 H70 B2 Mo N2 O3, C4 H8 O'
_chemical_formula_sum            'C59 H78 B2 Mo N2 O4'
_chemical_formula_weight         996.79
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-03
_audit_creation_method           'CIF-fill 1.4o (K.Radacki, 2005-23)'
_audit_update_record
;
2023-11-09 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.027(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1301(8)
_cell_length_b                   10.9095(4)
_cell_length_c                   24.8499(11)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.32
_cell_volume                     5178.9(4)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      -0,0393755
_diffrn_orient_matrix_UB_12      0,0571053
_diffrn_orient_matrix_UB_13      0,0070366
_diffrn_orient_matrix_UB_21      0,0196012
_diffrn_orient_matrix_UB_22      0,0616131
_diffrn_orient_matrix_UB_23      -0,0249068
_diffrn_orient_matrix_UB_31      -0,0283822
_diffrn_orient_matrix_UB_32      -0,0366731
_diffrn_orient_matrix_UB_33      -0,0308879
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13327
_diffrn_reflns_point_group_measured_fraction_full 0.499
_diffrn_reflns_point_group_measured_fraction_max 0.497
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.132
_diffrn_reflns_theta_min         1.066
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.745490
_exptl_absorpt_correction_T_min  .591966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofurane'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         13327
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0038P)^2^+27.6458P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                11687
_reflns_number_total             13327
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_cod_data_source_file            d3dt03787h2.cif
_cod_data_source_block           twin5_(DBA)Mo(CO)3
_cod_depositor_comments
'Adding full bibliography for 7714662--7714667.cif.'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7714664
_shelx_shelxl_version_number     2019/1
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in TWINABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_res_checksum              63340