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_4336791
_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         'C18 H39 Cl Co N3, C24 H20 B'
_chemical_formula_sum            'C42 H59 B Cl Co N3'
_chemical_formula_weight         711.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2013-05-28
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4655(11)
_cell_length_b                   11.4588(7)
_cell_length_c                   17.9216(11)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.121
_cell_measurement_theta_min      2.529
_cell_volume                     3792.1(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44421
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.138
_diffrn_reflns_theta_min         1.585
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0760 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.7642.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 8840 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         24098
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0650P)^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         0.1172
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.819
_reflns_number_gt                21532
_reflns_number_total             24098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402626p_si_002_10.cif
_cod_data_source_block           1305ThangavelttacnCoClBPh4
_cod_database_code               4336791
_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:
 C4B(H4BA,H4BB), C2(H2A,H2B), C5B(H5BA,H5BB), C1(H1A,H1B), C4(H4A,H4B), C3(H3A,
 H3B), C2B(H2BA,H2BB), C6B(H6BA,H6BB), C5(H5A,H5B), C6(H6A,H6B), C3B(H3BA,H3BB),
  C1B(H1BA,H1BB)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C33B(H33B), C39(H39), C42(H42), C30(H30), C40(H40), C36B(H36B),
 C24(H24), C38B(H38B), C28(H28), C39B(H39B), C41(H41), C20(H20), C21B(H21B),
 C21(H21), C26(H26), C27B(H27B), C34B(H34B), C20B(H20B), C24B(H24B), C32(H32),
 C32B(H32B), C35B(H35B), C36(H36), C27(H27), C38(H38), C34(H34), C28B(H28B),
 C33(H33), C30B(H30B), C41B(H41B), C40B(H40B), C35(H35), C42B(H42B), C22B(H22B),
  C29(H29), C29B(H29B), C23B(H23B), C26B(H26B), C23(H23)
2.c Idealised Me refined as rotating group:
 C14B(H14D,H14E,H14F), C9(H9A,H9B,H9C), C9B(H9BA,H9BB,H9BC), C12(H12A,H12B,
 H12C), C12B(H12D,H12E,H12F), C18(H18A,H18B,H18C), C18B(H18D,H18E,H18F),
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C13B(H13D,H13E,
 H13F), C13(H13A,H13B,H13C), C17B(H17D,H17E,H17F), C16B(H16D,H16E,H16F),
 C14(H14A,H14B,H14C), C10B(H10D,H10E,H10F), C8B(H8BA,H8BB,H8BC), C16(H16A,H16B,
 H16C)
;
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.738
_shelxl_version_number           2012-9