Insertion reactions of small unsaturated molecules in the N‒B bonds of boron guanidinates
Ramos, Alberto; Antiñolo, Antonio; Carrillo-Hermosilla, Fernando; Fernández-Galán, Rafael; Montero-Rama, María del Pilar; Villaseñor, Elena; Rodríguez-Diéguez, Antonio; García-Vivó, Daniel; Dalton Trans.  (2017) –; doi:10.1039/C7DT02081C

data_7043801
_publ_section_title
;
 Insertion reactions of small unsaturated molecules in the N--B bonds of
 boron guanidinates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02081C
_journal_year                    2017
_chemical_formula_moiety         'C49 H78 B2 N4 O'
_chemical_formula_sum            'C55 H92 B2 N4 O'
_chemical_formula_weight         846.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-07 deposited with the CCDC.
2017-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                69.089(3)
_cell_angle_beta                 85.835(3)
_cell_angle_gamma                75.449(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4481(18)
_cell_length_b                   14.078(2)
_cell_length_c                   16.683(2)
_cell_measurement_reflns_used    2878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.73
_cell_measurement_theta_min      2.39
_cell_volume                     2430.7(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21112
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        21.003
_diffrn_reflns_theta_max         21.003
_diffrn_reflns_theta_min         2.235
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0758 before and 0.0648 after correction. The Ratio of minimum to maximum transmission is 0.9138. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         5162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0781P)^2^+0.5111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3342
_reflns_number_total             5162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02081c3.cif
_cod_data_source_block           Compound10
_cod_database_code               7043801
_shelx_shelxl_version_number     2014/7
_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 Rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C49(H49A,
 H49B,H49C)
2.b Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C25(H25), C31(H31), C37(H37), C40(H40)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
2.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C19(H19), C20(H20), C44(H44), C45(H45), C47(H47), C48(H48)
;
_shelx_res_checksum              9647
_shelx_fab_checksum              7937
_olex2_submission_special_instructions 'No special instructions were received'