X-ray Crystallography Analysis of Complexes Synthesized with Tris(2-pyridylmethyl)amine: A Laboratory Experiment for Undergraduate Students Integrating Interdisciplinary Concepts and Techniques
Bazley, Isabel J.; Erie, Ellen A.; Feiereisel, Garrett M.; LeWarne, Christopher J.; Peterson, Jack M.; Sandquist, Katherine L.; Oshin, Kayode D.; Zeller, Matthias; Journal of Chemical Education  (2018) –; doi:10.1021/acs.jchemed.7b00685

data_1549067
_publ_section_title
;
 X-ray Crystallography Analysis of Complexes Synthesized with
 Tris(2-pyridylmethyl)amine: A Laboratory Experiment for Undergraduate
 Students Integrating Interdisciplinary Concepts and Techniques
;
_journal_name_full               'Journal of Chemical Education'
_journal_paper_doi               10.1021/acs.jchemed.7b00685
_journal_year                    2018
_chemical_formula_moiety         '0.5(C18 H19 N4), 0.5(C18 H18 N4)'
_chemical_formula_sum            'C18 H18.5 N4'
_chemical_formula_weight         290.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4860)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3233(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.1903(3)
_cell_length_b                   35.9841(18)
_cell_length_c                   14.2498(7)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.69
_cell_volume                     3140.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      119.99
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66915
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7056
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0417 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.9462.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2302
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1236.4133
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.054
_refine_diff_density_max         3.7023
_refine_diff_density_min         -1.1838
_refine_diff_density_rms         0.2006
_refine_ls_d_res_high            0.7466
_refine_ls_d_res_low             17.9921
_refine_ls_goodness_of_fit_ref   4.0807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    67
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      4.0807
_refine_ls_R_factor_all          0.2028
_refine_ls_R_factor_gt           0.1748
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4848
_refine_ls_wR_factor_ref         0.5057
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -6
_reflns_number_gt                6058
_reflns_number_total             7876
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            TPMA.cif
_cod_data_source_block           KO_TPMA
_cod_database_code               1549067
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C19(H19a,H19b), C38(H38a,H38b), C40(H40a,H40b)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C42(H42), C39(H39), C5(H5), C23(H23), C32(H32), C15(H15), C12(H12),
 C30(H30), C21(H21), C18(H18), C1(H1), C26(H26), C24(H24), C25(H25), C3(H3),
 C29(H29), C31(H31), C22(H22), C4(H4), C14(H14), C20(H20), C27(H27), C33(H33),
 C43(H37)
;
_olex2_submission_special_instructions 'No special instructions were received'