Amido Ca(ii) complexes supported by Schiff base ligands for catalytic cross-dehydrogenative coupling of amines with silanes.
Forosenko, Natalia V.; Basalov, Ivan V.; Cherkasov, Anton V.; Fukin, Georgy K.; Shubina, Elena S.; Trifonov, Alexander A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12570–12581; doi:10.1039/c8dt01130c

data_7701924
_publ_section_title
;
 Amido Ca(ii) complexes supported by Schiff base ligands for catalytic
 cross-dehydrogenative coupling of amines with silanes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12570
_journal_page_last               12581
_journal_paper_doi               10.1039/c8dt01130c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C38 H61 Ca N3 O3 Si2'
_chemical_formula_sum            'C38 H61 Ca N3 O3 Si2'
_chemical_formula_weight         704.15
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1zgjkj
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-03-20 deposited with the CCDC.	2019-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                74.996(2)
_cell_angle_beta                 86.375(2)
_cell_angle_gamma                88.424(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7618(10)
_cell_length_b                   12.4539(13)
_cell_length_c                   15.7229(15)
_cell_measurement_reflns_used    4708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.26
_cell_volume                     2031.2(3)
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27526
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.940
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: L. Krause et al., J. Appl. Cryst., 2015, 48, 3-10
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.4560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7331
_reflns_number_total             9719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01130c2.cif
_cod_data_source_block           loqcan
_cod_database_code               7701924
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              49155