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_7123805
_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            'C45 H77 B Ca N4 O'
_chemical_formula_weight         741.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.731(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5271(7)
_cell_length_b                   18.2281(10)
_cell_length_c                   12.1212(7)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.28
_cell_volume                     2259.5(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37048
_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         27.505
_diffrn_reflns_theta_min         2.826
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_meas      1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6495
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 3596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.028(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0357P)^2^+0.3576P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                8614
_reflns_number_total             10388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04698d2.cif
_cod_data_source_block           complex_4
_cod_original_formula_sum        '	C45 H77 B Ca N4 O'
_cod_database_code               7123805
_shelx_estimated_absorpt_t_min   0.6495
_shelx_estimated_absorpt_t_max   0.7456
_shelxl_version_number           2013-2
_shelx_res_checksum              97439