Smart composite films of nanometric thickness based on copper-iodine coordination polymers. Toward sensors.
Conesa-Egea, Javier; Nogal, Noemí; Martínez, José Ignacio; Fernández-Moreira, Vanesa; Rodríguez-Mendoza, Ulises R; González-Platas, Javier; Gómez-García, Carlos J; Delgado, Salomé; Zamora, Félix; Amo-Ochoa, Pilar; Chemical science 9 (2018) 8000–8010; doi:10.1039/c8sc03085e

data_1549827
_publ_section_title
;
 Smart composite films of nanometric thickness based on copper-iodine
 coordination polymers. Toward sensors.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              8000
_journal_page_last               8010
_journal_paper_doi               10.1039/c8sc03085e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C7 H8 Cu I N2 O2'
_chemical_formula_sum            'C7 H8 Cu I N2 O2'
_chemical_formula_weight         342.59
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                87.71(2)
_cell_angle_beta                 88.616(15)
_cell_angle_gamma                87.10(3)
_cell_formula_units_Z            2
_cell_length_a                   3.9759(7)
_cell_length_b                   8.862(3)
_cell_length_c                   10.6257(17)
_cell_measurement_reflns_used    1136
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      24.4340
_cell_measurement_theta_min      3.8150
_cell_volume                     373.52(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 (Sheldrick, 2015)'
_diffrn_ambient_pressure         6670000(40000)
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.357
_diffrn_measured_fraction_theta_max 0.357
_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    -23.00  10.00   0.50   40.00    --   -0.31  67.00 -23.00   66
  2  \w    -41.00  11.00   0.50   40.00    --   29.92  13.00  -3.00  104
  3  \w    -17.00  15.00   0.50   40.00    --   29.92  39.00 -12.00   64
  4  \w     48.00  96.00   0.50   40.00    --   29.92-134.00-123.00   96
  5  \w    -42.00 -17.00   0.50   40.00    --   29.92 134.00 123.00   50
  6  \w    -22.00   4.00   0.50   40.00    --   29.92  97.00 -35.00   52
  7  \w     -1.00  48.00   0.50   40.00    --   29.92 -67.00  23.00   98
  8  \w    -15.00  51.00   0.50   40.00    --   29.92 -53.00-162.00  132
  9  \w    -13.00  11.00   0.50   40.00    --   29.92  81.00 151.00   48
 10  \w    -42.00  12.00   0.50   40.00    --   29.92  26.00 172.00  108
 11  \w    -42.00 -17.00   0.50   40.00    --   29.92 134.00 -57.00   50
 12  \w    -22.00  13.00   0.50   40.00    --  -30.54 -39.00-167.00   70
 13  \w     -9.00  37.00   0.50   40.00    --  -30.54 -26.00-172.00   92
 14  \w    -69.00 -21.00   0.50   40.00    --  -30.54  97.00 -35.00   96
 15  \w    -50.00  18.00   0.50   40.00    --  -30.54  39.00 167.00  136
 16  \w    -17.00  16.00   0.50   40.00    --  -30.54 -39.00  12.00   66
 17  \w    -16.00   5.00   0.50   40.00    --  -30.54 -67.00  23.00   42
 18  \w      1.00  36.00   0.50   40.00    --  -30.54 -26.00   7.00   70
 19  \w    -41.00  -2.00   0.50   40.00    --  -30.54  13.00  -3.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0063065000
_diffrn_orient_matrix_UB_12      -0.0795348000
_diffrn_orient_matrix_UB_13      0.0111291000
_diffrn_orient_matrix_UB_21      0.1721320000
_diffrn_orient_matrix_UB_22      -0.0038585000
_diffrn_orient_matrix_UB_23      -0.0193208000
_diffrn_orient_matrix_UB_31      0.0474778000
_diffrn_orient_matrix_UB_32      0.0095709000
_diffrn_orient_matrix_UB_33      0.0629935000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.357
_diffrn_reflns_Laue_measured_fraction_max 0.357
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2384
_diffrn_reflns_point_group_measured_fraction_full 0.357
_diffrn_reflns_point_group_measured_fraction_max 0.357
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         3.839
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.014
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.046
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.942
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+17.3416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                409
_reflns_number_total             473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03085e2.cif
_cod_data_source_block           JCE140CS_667GPa
_cod_depositor_comments
'Adding full bibliography for 1549820--1549832.cif.'
_cod_database_code               1549827
_shelx_shelxl_version_number     2017/1
_exptl_oxdiff_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are:
         range of dac transmission factors (min-max)      0.276     0.352
         range of gasket transmission (min-max)           0.995     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 15.500 mm, mu =  0.0202 mm-1
       thickness of platten 1: 44.000 mm, mu =  0.0047 mm-1

 thickness of diamond anvil 2: 15.500 mm, mu =  0.0202 mm-1
       thickness of platten 2: 44.000 mm, mu =  0.0047 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness =  50.0 microns, radius = 105.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_reflns_odcompleteness_completeness 35.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cu1) = Uanis(I1)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2)
3.b Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1)
3.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_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 1.963
_oxdiff_exptl_absorpt_empirical_full_min 0.633