Molecular self-assembly of 1D infinite polyiodide helices in a phenanthrolinium salt.
Poręba, Tomasz; Swiątkowski, Marcin; Kruszyński, Rafał; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2800–2806; doi:10.1039/d0dt04042h

data_7706514
_publ_section_title
;
 Molecular self-assembly of 1D infinite polyiodide helices in a
 phenanthrolinium salt.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2800
_journal_page_last               2806
_journal_paper_doi               10.1039/d0dt04042h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'I7, 3(C12 H8 N2), 3(C12 H9 N2)'
_chemical_formula_sum            'C72 H51 I7 N12'
_chemical_formula_weight         1972.55
_chemical_melting_point          363
_chemical_name_common
'poly-[tris(1,10-phenanthrolin-1-ium 1,10-phenanthroline) heptaiodide]'
_chemical_name_systematic
'poly-[tris(1,10-phenanthrolin-1-ium 1,10-phenanthroline) heptaiodide]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0054(3)
_cell_length_b                   12.4116(2)
_cell_length_c                   22.5277(5)
_cell_measurement_reflns_used    17987
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.5980
_cell_measurement_theta_min      3.9850
_cell_volume                     6712.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -96.00 -16.00   0.50    1.00    --  -86.25 125.00 -30.00  160
  2  \w     33.00  71.00   0.50    1.00    --  107.75 -38.00-180.00   76
  3  \w     33.00  71.00   0.50    1.00    --  107.75 -38.00  60.00   76
  4  \w     40.00  70.00   0.50    1.00    --  107.75 -38.00  30.00   60
  5  \w     33.00  71.00   0.50    1.00    --  107.75 -38.00 150.00   76
  6  \w     83.00 128.00   0.50    1.00    --  107.75 -77.00  90.00   90
  7  \w     39.00 111.00   0.50    1.00    --  107.75 -99.00 120.00  144
  8  \w     57.00 121.00   0.50    0.50    --   49.71-178.00  90.00  128
  9  \w     98.00 178.00   0.50    1.00    --  107.75  38.00  60.00  160
 10  \w    -71.00 -11.00   0.50    1.00    --  -86.25  38.00   0.00  120
 11  \w   -120.00   7.00   0.50    0.50    --  -49.71   0.00 120.00  254
 12  \w   -120.00 -38.00   0.50    0.50    --  -49.71-178.00-150.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0592675000
_diffrn_orient_matrix_UB_12      -0.0463662000
_diffrn_orient_matrix_UB_13      -0.0056125000
_diffrn_orient_matrix_UB_21      0.0244469000
_diffrn_orient_matrix_UB_22      0.1128090000
_diffrn_orient_matrix_UB_23      0.0115551000
_diffrn_orient_matrix_UB_31      0.0007080000
_diffrn_orient_matrix_UB_32      -0.0234227000
_diffrn_orient_matrix_UB_33      0.0671961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32488
_diffrn_reflns_point_group_measured_fraction_full 0.794
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         3.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    25.833
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       needle
_exptl_crystal_F_000             3752
_exptl_crystal_recrystallization_method
'double-layer slow liquid-liquid diffusion'
_exptl_crystal_size_max          0.793
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.242
_refine_diff_density_min         -2.371
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 2953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9743
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0232P)^2^+81.9529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.546
_reflns_Friedel_fraction_full    0.579
_reflns_Friedel_fraction_max     0.575
_reflns_number_gt                9045
_reflns_number_total             9743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04042h2.cif
_cod_data_source_block           linear_polyiodide
_cod_depositor_comments          'Adding full bibliography for 7706514.cif.'
_cod_database_code               7706514
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         ' C30 H24 N6 I7'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6C-C12C
 1.38 with sigma of 0.02
 C11C-C5C
 1.38 with sigma of 0.02
 C1E-C11E
 1.38 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6D) = Uanis(C5D) = Uanis(C11D) = Uanis(C4D) = Uanis(C3D) = Uanis(C2D) =
Uanis(C1D) = Uanis(C10D) = Uanis(C12D) = Uanis(C7D) = Uanis(C8D) = Uanis(C9D)
Uanis(C2E) = Uanis(C3E) = Uanis(C4E) = Uanis(C11E) = Uanis(C1E) = Uanis(C5E) =
Uanis(C6E) = Uanis(C12E) = Uanis(C10E) = Uanis(C7E) = Uanis(C8E) = Uanis(C9E)
Uanis(C2F) = Uanis(C3F) = Uanis(C4F) = Uanis(C11F) = Uanis(C1F) = Uanis(C5F) =
Uanis(C6F) = Uanis(C12F) = Uanis(C10F) = Uanis(C7F) = Uanis(C8F) = Uanis(C9F)
Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C12) = Uanis(C10) = Uanis(C1) =
Uanis(C6) = Uanis(C5) = Uanis(C11) = Uanis(C2) = Uanis(C3) = Uanis(C4)
Uanis(C9B) = Uanis(C8B) = Uanis(C7B) = Uanis(C12B) = Uanis(C6B) = Uanis(C5B) =
Uanis(C11B) = Uanis(C4B) = Uanis(C3B) = Uanis(C2B) = Uanis(C1B) = Uanis(C10B)
Uanis(C9C) = Uanis(C8C) = Uanis(C7C) = Uanis(C12C) = Uanis(C10C) = Uanis(C6C) =
Uanis(C5C) = Uanis(C11C) = Uanis(C4C) = Uanis(C1C) = Uanis(C2C) = Uanis(C3C)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N1B(H1B), N1C(H1C), C4(H4), C5(H5), C4B(H4B), C7F(H7F), C9F(H9F),
 C7(H7), C2E(H2E), C2F(H2F), C8F(H8F), C9E(H9E), C3F(H3F), C9D(H9D), C5D(H5D),
 C8(H8), C2D(H2D), C4F(H4F), C6(H6), C8D(H8D), C7B(H7B), C8C(H8C), C8E(H8E),
 C2(H2), C6B(H6B), C5C(H5C), C2B(H2B), C7E(H7E), C5B(H5B), C4E(H4E), C3(H3),
 C9(H9), C4C(H4C), C3C(H3C), C7D(H7D), C5E(H5E), C3B(H3B), C6F(H6F), C2C(H2C),
 C5F(H5F), C3E(H3E), C6C(H6C), C9C(H9C), C8B(H8B), C3D(H3D), C9B(H9B), C6E(H6E),
  C6D(H6D), C4D(H4D), C7C(H7C)
;
_shelx_res_checksum              87594
_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 1.511
_oxdiff_exptl_absorpt_empirical_full_min 0.735