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_7123808
_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_moiety         'C39 H69 B Ca N4 O'
_chemical_formula_sum            'C39 H69 B Ca N4 O'
_chemical_formula_weight         660.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 106.1440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6088(4)
_cell_length_b                   15.1912(7)
_cell_length_c                   21.9255(8)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.35
_cell_volume                     4034.1(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63556
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.151
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_meas      1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.978
_exptl_transmission_factor_min   0.965
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9279
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0774P)^2^+4.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5957
_reflns_number_total             9279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04698d2.cif
_cod_data_source_block           complex_6
_cod_original_formula_sum        '	C39 H69 B Ca N4 O'
_cod_database_code               7123808
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              22455