Group 2 metal (Mg, Ca, Sr) silylamides supported by a cyclen-derived macrocyclic polyamine
Mukherjee, Debabrata; Shirase, Satoru; Beckerle, Klaus; Spaniol, Thomas Paul; Mashima, Kazushi; Okuda, Jun; Dalton Trans.  (2017) –; doi:10.1039/C7DT01727H

data_7043216
_publ_section_title
;
 Group 2 metal (Mg, Ca, Sr) silylamides supported by a cyclen-derived
 macrocyclic polyamine
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01727H
_journal_year                    2017
_chemical_formula_moiety         'C21 H56 N6 Si4 Sr'
_chemical_formula_sum            'C21 H56 N6 Si4 Sr'
_chemical_formula_weight         592.69
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6835(18)
_cell_length_b                   17.274(3)
_cell_length_c                   17.745(3)
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.23
_cell_volume                     3274.8(10)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.1437
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10065
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf and pentane'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 1499 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.092(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0572
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                4488
_reflns_number_total             6158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01727h2.cif
_cod_data_source_block           4
_cod_database_code               7043216
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.799
_shelxl_version_number           2013-4
_shelx_res_checksum              48390