Polymerization Studies of Diiodohexatriyne and Diiodooctatetrayne Cocrystals
Freitag, Matthew; DeCicco, Racquel C.; Black, Allison; Ang, Xiuzhu; Young, Christopher N.; Resch, Daniel; Halada, Gary P.; Phillips, Brian L.; Goroff, Nancy S.; Macromolecules 52 (2019) 8563–; doi:10.1021/acs.macromol.9b00960

data_1552745
_publ_section_title
;
 Polymerization Studies of Diiodohexatriyne and Diiodooctatetrayne
 Cocrystals
;
_journal_issue                   22
_journal_name_full               Macromolecules
_journal_page_first              8563
_journal_paper_doi               10.1021/acs.macromol.9b00960
_journal_volume                  52
_journal_year                    2019
_chemical_formula_moiety         'C6 I2, C8 H13 N2 O'
_chemical_formula_sum            'C14 H13 I2 N2 O'
_chemical_formula_weight         479.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2008-09-02
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:32:32, GUI svn.r4372)
;
_cell_angle_alpha                90.740(5)
_cell_angle_beta                 94.177(4)
_cell_angle_gamma                96.566(5)
_cell_formula_units_Z            2
_cell_length_a                   5.1369(3)
_cell_length_b                   8.3240(6)
_cell_length_c                   19.8365(10)
_cell_measurement_reflns_used    3733
_cell_measurement_theta_max      24.4840
_cell_measurement_theta_min      3.8740
_cell_volume                     840.20(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4962
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8835
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -22.00  87.00   1.00   19.48    --   10.71  77.00-120.00  109
  2  \w    -40.00  62.00   1.00   19.48    --  -11.57  57.00 120.00  102
  3  \w    -84.00  17.00   1.00   19.48    --  -11.57 -57.00 -30.00  101
  4  \w     34.00  99.00   1.00   19.48    --   10.71 179.00  90.00   65
  5  \w      1.00  70.00   1.00   19.48    --   10.71-132.00 -95.00   69
  6  \w    -86.00  13.00   1.00   19.48    --  -11.57 -37.00  60.00   99
  7  \w    -40.00  62.00   1.00   19.48    --  -11.57  57.00   0.00  102
  8  \w    -71.00 -22.00   1.00   19.48    --  -11.57 132.00 -26.00   49
  9  \w    -99.00 -53.00   1.00   19.48    --  -11.57 179.00 150.00   46
 10  \w    -25.00   0.00   1.00   19.48    --   10.71 -99.00 -60.00   25
 11  \w    -75.00 -26.00   1.00   19.48    --  -11.57 137.00 150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0150622000
_diffrn_orient_matrix_UB_12      0.0757482000
_diffrn_orient_matrix_UB_13      0.0174829000
_diffrn_orient_matrix_UB_21      -0.0011782000
_diffrn_orient_matrix_UB_22      0.0402291000
_diffrn_orient_matrix_UB_23      -0.0313059000
_diffrn_orient_matrix_UB_31      -0.1385591000
_diffrn_orient_matrix_UB_32      -0.0020850000
_diffrn_orient_matrix_UB_33      -0.0005320000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18625
_diffrn_reflns_theta_full        29.8788
_diffrn_reflns_theta_max         29.88
_diffrn_reflns_theta_min         3.25
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.8935
_exptl_crystal_F_000             448.5159
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.4544
_refine_diff_density_min         -1.0403
_refine_diff_density_rms         0.2449
_refine_ls_d_res_high            0.7133
_refine_ls_d_res_low             6.2771
_refine_ls_goodness_of_fit_ref   1.0279
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0279
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.0070
_refine_ls_shift/su_mean         0.0012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                2441
_reflns_number_total             4284
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ma9b00960_si_002.cif
_cod_data_source_block           exp_3425
_cod_depositor_comments
'Adding full bibliography for 1552745--1552747.cif.'
_cod_original_cell_volume        840.22(9)
_cod_database_code               1552745
_chemical_oxdiff_formula         'C28 H26 I4 N4 O2 '
_chemical_oxdiff_usercomment     'C6I2*6MO co-crystal fresh'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H9 of N9, {H12a,H12b} of C12, {H13a,H13b} of C13, {H16a,H16b} of C16, {H15a,
  H15b} of C15, {H17a,H17b} of C17, {H14a,H14b} of C14
2.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C13(H13a,H13b), C16(H16a,H16b), C15(H15a,H15b), C17(H17a,
 H17b), C14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 N9(H9)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.152
_oxdiff_exptl_absorpt_empirical_full_min 0.381