Monodentate coordination of the normally chelating chiral diamine (R,R)-TMCDA.
Ojeda-Amador, Ana I; Martínez-Martínez, Antonio J; Kennedy, Alan R.; Armstrong, David R.; O'Hara, Charles T; Chemical communications (Cambridge, England) 53 (2016) 324–327; doi:10.1039/c6cc07190b

data_7119216
_publ_section_title
;
 Monodentate coordination of the normally chelating chiral diamine
 (R,R)-TMCDA.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              324
_journal_page_last               327
_journal_paper_doi               10.1039/c6cc07190b
_journal_volume                  53
_journal_year                    2016
_chemical_formula_moiety         'C32 H80 N6 Na2 Si4'
_chemical_formula_sum            'C32 H80 N6 Na2 Si4'
_chemical_formula_weight         707.36
_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   geom
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;
2016-08-31 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6278(4)
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_cell_length_c                   32.841(2)
_cell_measurement_reflns_used    6122
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_cell_measurement_theta_min      3.0780
_cell_volume                     4531.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXLE (Hubschle, Sheldrick and Dittrich)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
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_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_limit_k_max       16
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_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            25854
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_min         2.748
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99322
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 3292 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         11578
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0439P)^2^+0.1903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.756
_reflns_number_gt                9541
_reflns_number_total             11578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07190b2.cif
_cod_data_source_block           amao450smart_disorder
_cod_database_code               7119216
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81287
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