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_1552746
_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         '2(C6 I2), C16 H26 N4 O2'
_chemical_formula_sum            'C28 H26 I4 N4 O2'
_chemical_formula_weight         958.16
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90.726(6)
_cell_angle_beta                 96.620(5)
_cell_angle_gamma                90.949(5)
_cell_formula_units_Z            1
_cell_length_a                   4.8910(2)
_cell_length_b                   8.2349(6)
_cell_length_c                   20.7211(15)
_cell_measurement_reflns_used    2516
_cell_measurement_theta_max      26.4580
_cell_measurement_theta_min      3.8030
_cell_volume                     828.81(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4962
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.8553
_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    -13.00  84.50   0.75   33.83    --   10.94  37.00-120.00  130
  2  \w    -25.00  29.00   0.75   33.83    --  -11.72 -99.00-120.00   72
  3  \w    -53.00  67.00   0.75   33.83    --  -11.72  19.00  60.00  160
  4  \w    -25.00   2.00   0.75   33.83    --   10.94 -99.00  90.00   36
  5  \w    -86.00  13.00   0.75   33.83    --  -11.72 -37.00  30.00  132
  6  \w    -40.00  60.50   0.75   33.83    --  -11.72  57.00-180.00  134
;
_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      0.0266758000
_diffrn_orient_matrix_UB_12      -0.0505155000
_diffrn_orient_matrix_UB_13      0.0274028000
_diffrn_orient_matrix_UB_21      0.0005302000
_diffrn_orient_matrix_UB_22      -0.0688852000
_diffrn_orient_matrix_UB_23      -0.0208790000
_diffrn_orient_matrix_UB_31      0.1435722000
_diffrn_orient_matrix_UB_32      0.0112308000
_diffrn_orient_matrix_UB_33      -0.0009586000
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11194
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.85
_diffrn_reflns_theta_min         3.84
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.9195
_exptl_crystal_F_000             448.2739
_exptl_crystal_size_max          0.878
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.022
_refine_diff_density_max         2.8152
_refine_diff_density_min         -1.8057
_refine_diff_density_rms         0.3275
_refine_ls_d_res_high            0.7140
_refine_ls_d_res_low             5.3088
_refine_ls_goodness_of_fit_ref   1.0394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0394
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+10.5882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                2452
_reflns_number_total             4079
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ma9b00960_si_003.cif
_cod_data_source_block           exp_3467
_cod_depositor_comments
'Adding full bibliography for 1552745--1552747.cif.'
_cod_database_code               1552746
_chemical_oxdiff_formula         'C28 H26 I4 N4 O2'
_chemical_oxdiff_usercomment     PIEDA
_reflns_odcompleteness_completeness 49.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C(Ha,Hb), C3AA(H3Aa,H3Ab), C4AA(H4Aa,H4Ab), C5(H5a,H5b), C2AA(H2Aa,H2Ab),
 C2(H2a,H2b)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.041
_oxdiff_exptl_absorpt_empirical_full_min 0.537