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_1549829
_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                87.474(16)
_cell_angle_beta                 88.623(8)
_cell_angle_gamma                86.839(17)
_cell_formula_units_Z            2
_cell_length_a                   3.9890(4)
_cell_length_b                   8.933(3)
_cell_length_c                   10.6670(10)
_cell_measurement_reflns_used    905
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      24.9260
_cell_measurement_theta_min      3.8100
_cell_volume                     379.07(14)
_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         6000000(40000)
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2536
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.356
_diffrn_measured_fraction_theta_max 0.356
_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      2.00  49.00   0.50   35.00    --   26.48 -39.00-167.00   94
  2  \w    -46.00 -17.00   0.50   35.00    --   26.48 134.00 -57.00   58
  3  \w    -43.00 -17.00   0.50   35.00    --   26.48 134.00 123.00   52
  4  \w    -20.00   5.00   0.50   35.00    --   26.48  39.00 -12.00   50
  5  \w    -27.00  17.00   0.50   35.00    --  -27.10 -39.00  12.00   88
  6  \w    -27.00  20.00   0.50   35.00    --  -27.10 -39.00-167.00   94
  7  \w    -11.00  14.00   0.50   35.00    --  -27.10 -81.00  29.00   50
  8  \w    -11.00  16.00   0.50   35.00    --  -27.10  39.00 167.00   54
  9  \w    -68.00  -1.00   0.50   35.00    --  -27.10  81.00 -29.00  134
 10  \w    -14.00  19.00   0.50   35.00    --  -27.10   0.00   0.00   66
 11  \w    -75.00 -16.00   0.50   35.00    --  -27.10  97.00 143.00  118
 12  \w    -52.00 -16.00   0.50   35.00    --  -27.10  39.00 167.00   72
 13  \w    -11.00  14.00   0.50   35.00    --  -27.10 -81.00-151.00   50
;
_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      0.0072619000
_diffrn_orient_matrix_UB_12      -0.0788945000
_diffrn_orient_matrix_UB_13      0.0115878000
_diffrn_orient_matrix_UB_21      0.1712088000
_diffrn_orient_matrix_UB_22      -0.0039093000
_diffrn_orient_matrix_UB_23      -0.0197424000
_diffrn_orient_matrix_UB_31      0.0486131000
_diffrn_orient_matrix_UB_32      0.0097596000
_diffrn_orient_matrix_UB_33      0.0625157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.356
_diffrn_reflns_Laue_measured_fraction_max 0.356
_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            1860
_diffrn_reflns_point_group_measured_fraction_full 0.356
_diffrn_reflns_point_group_measured_fraction_max 0.356
_diffrn_reflns_theta_full        25.003
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.911
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.230
_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    3.001
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0497P)^2^+16.3097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                413
_reflns_number_total             478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03085e2.cif
_cod_data_source_block           JCE140CS_600GPa
_cod_depositor_comments
'Adding full bibliography for 1549820--1549832.cif.'
_cod_original_cell_volume        379.09(12)
_cod_database_code               1549829
_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)      0.280     0.352
         range of gasket transmission (min-max)           0.996     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 35.65
_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 1.711
_oxdiff_exptl_absorpt_empirical_full_min 0.618