Stoichiometric reactions and catalytic dehydrogenations of amine-boranes with calcium aryloxide
Zheng, Xizhou; Huang, Jiasu; Yao, Yingming; Xu, Xin; Chemical Communications  (2019) –; doi:10.1039/C9CC04698D

data_7123806
_publ_section_title
;
 Stoichiometric reactions and catalytic dehydrogenations of amine-boranes
 with calcium aryloxide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04698D
_journal_year                    2019
_chemical_formula_sum            'C47 H69 B Ca N4 O'
_chemical_formula_weight         756.95
_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_method           SHELXL-2018/3
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                89.9400(10)
_cell_angle_beta                 76.5340(10)
_cell_angle_gamma                79.1860(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3589(4)
_cell_length_b                   12.5204(4)
_cell_length_c                   16.7864(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.39
_cell_volume                     2278.19(14)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0707
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         1.879
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS-2016/2 - Bruker AXS area detector '
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+1.9008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7559
_reflns_number_total             10465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04698d2.cif
_cod_data_source_block           complex_5
_cod_original_formula_sum        '	C47 H69 B Ca N4 O'
_cod_database_code               7123806
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              84666