1,4,7-Triazacyclononane Ligands Bearing Tertiary Alkyl Nitrogen Substituents
Arumugam Thangavel; Marika Wieliczko; John Bacsa; Christopher C. Scarborough; Inorganic Chemistry 52 (2013) 13282–13287; doi:10.1021/ic402626p

data_4336785
_publ_contact_author_address
; 
Department of Chemistry
Emory University
Atlanta, GA 30322, USA
;
_publ_contact_author_email       scarborough@emory.edu
_publ_contact_author_name        'Scarborough, Christopher C.'
_publ_section_title
;
 1,4,7-Triazacyclononane Ligands Bearing Tertiary Alkyl Nitrogen
 Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13282
_journal_page_last               13287
_journal_paper_doi               10.1021/ic402626p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C24 H20 B, C18 H39 Fe I N3, 0.5(C2 H3 N)'
_chemical_formula_sum            'C43 H60.5 B Fe I N3.5'
_chemical_formula_weight         820.01
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2012-08-25
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Aug 15 2012 15:59:22, GUI svn.r4314)
;
_cell_angle_alpha                71.5257(14)
_cell_angle_beta                 86.7503(14)
_cell_angle_gamma                81.4313(14)
_cell_formula_units_Z            8
_cell_length_a                   20.0457(19)
_cell_length_b                   20.160(2)
_cell_length_c                   21.249(2)
_cell_measurement_reflns_used    9258
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.424
_cell_measurement_theta_min      2.299
_cell_volume                     8053.3(13)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            128372
_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         28.487
_diffrn_reflns_theta_min         1.027
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1015 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.7071.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             3415
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.194
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1821
_refine_ls_number_reflns         40620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+4.5451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24595
_reflns_number_total             40620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402626p_si_002_04.cif
_cod_data_source_block           1209_ThangavelttacnFeIBPh4MeCN
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C86 H121 B2 Fe2 I2 N7'
_cod_original_formula_weight         1640.02
_cod_original_formula_moiety       '2(C24 H20 B), 2(C18 H39 Fe I N3), C2 H3 N'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        8053.1(14)
_cod_database_code               4336785
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C1C(H1CA,H1CB), C3B(H3BA,H3BB), C2B(H2BA,H2BB), C4B(H4BA,H4BB),
 C6B(H6BA,H6BB), C5B(H5BA,H5BB), C1D(H1DA,H1DB), C2C(H2CA,H2CB), C4C(H4CA,H4CB),
  C5C(H5CA,H5CB), C6C(H6CA,H6CB), C3C(H3CA,H3CB), C2D(H2DA,H2DB), C4D(H4DA,
 H4DB), C1E(H1EA,H1EB), C3D(H3DA,H3DB), C6D(H6DA,H6DB), C5D(H5DA,H5DB)
2.b Aromatic/amide H refined with riding coordinates:
 C82(H82), C77(H77), C84(H84), C90(H90), C80(H80), C94(H94), C97(H97),
 C93(H93), C81(H81), C92(H92), C96(H96), C88(H88), C86(H86), C99(H99),
 C100(H100), C87(H87), C91(H91), C85(H85), C79(H79), C98(H98), C88D(H88D),
 C98D(H98D), C1(H1), C92D(H92D), C99D(H99D), C93D(H93D), C84D(H84D), C91D(H91D),
  C96D(H96D), C87D(H87D), C94D(H94D), C85D(H85D), C80D(H80D), C82D(H82D),
 C97D(H97D), C81D(H81D), C79D(H79D), C77D(H77D), C90D(H90D), C86D(H86D),
 C93C(H93C), C94C(H94C), C82C(H82C), C87C(H87C), C84C(H84C), C79C(H79C),
 C81C(H81C), C80C(H80C), C97C(H97C), C90C(H90C), C88C(H88C), C99C(H99C),
 C86C(H86C), C91C(H91C), C2(H2), C85C(H85C), C77C(H77C), C92C(H92C), C96C(H96C),
  C98C(H98C), C86B(H86B), C84B(H84B), C98B(H98B), C81B(H81B), C3(H3),
 C90B(H90B), C92B(H92B), C82B(H82B), C87B(H87B), C91B(H91B), C93B(H93B),
 C77B(H77B), C97B(H97B), C96B(H96B), C94B(H94B), C99B(H99B), C85B(H85B),
 C79B(H79B), C88B(H88B), C80B(H80B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C9(H9A,H9B,H9C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C1A(H1AA,H1AB,H1AC), C16B(H16D,H16E,H16F), C12B(H12D,H12E,H12F),
 C8B(H8BA,H8BB,H8BC), C18B(H18D,H18E,H18F), C17B(H17D,H17E,H17F), C13B(H13A,
 H13B,H13C), C10B(H10C,H10D,H10E), C9B(H9BA,H9BB,H9BC), C14B(H14D,H14E,H14F),
 C13C(H13D,H13E,H13F), C17C(H17G,H17H,H17I), C8C(H8CA,H8CB,H8CC), C18C(H18G,
 H18H,H18I), C9C(H9CA,H9CB,H9CC), C10C(H10F,H10G,H10H), C14C(H14G,H14H,H14I),
 C12C(H12G,H12H,H12I), C16C(H16G,H16H,H16I), C18D(H18J,H18K,H18L), C12D(H12J,
 H12K,H12L), C9D(H9DA,H9DB,H9DC), C17D(H17J,H17K,H17L), C16D(H16J,H16K,H16L),
 C14D(H14J,H14K,H14L), C8D(H8DA,H8DB,H8DC), C10D(H10I,H10J,H10K), C13D(H13G,
 H13H,H13I), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C)
;
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.643
_shelxl_version_number           2013-4