Hybrid Organic-Inorganic Coordination Complexes as Tunable Optical Response Materials.
Travis, Will; Knapp, Caroline E.; Savory, Christopher N.; Ganose, Alex M.; Kafourou, Panagiota; Song, Xingchi; Sharif, Zainab; Cockcroft, Jeremy K.; Scanlon, David O.; Bronstein, Hugo; Palgrave, Robert G.; Inorganic chemistry 55 (2016) 3393–3400; doi:10.1021/acs.inorgchem.5b02749

data_4347119
_publ_section_title
;
 Hybrid Organic-Inorganic Coordination Complexes as Tunable Optical
 Response Materials.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3393
_journal_page_last               3400
_journal_paper_doi               10.1021/acs.inorgchem.5b02749
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.25(C72 H40 I8 N16 Pb4)'
_chemical_formula_sum            'C18 H10 I2 N4 Pb'
_chemical_formula_weight         743.29
_chemical_name_systematic        'lead diiodide dipyridophenazine'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
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_cell_length_b                   15.9159(3)
_cell_length_c                   14.4471(3)
_cell_measurement_temperature    99
_cell_volume                     1881.20(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
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;
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omega____ theta____ kappa____ phi______ frames
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  2 omega  -67.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -56.00  -10.00   1.0000    1.0000
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  4 omega  -74.00  -23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega  -87.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega    1.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega    1.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega    2.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   47.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   91.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 11 omega   96.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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omega____ theta____ kappa____ phi______ frames
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 17 omega   37.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 18 omega   38.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 19 omega   37.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 20 omega   84.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   90.0000 29

 21 omega  118.00  174.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   60.0000 56

 22 omega  152.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 23 omega  140.00  166.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 24 omega  127.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 51

 25 omega  116.00  177.00   1.0000    1.0000
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    -      112.0000   73.0000  -97.4918 61

 26 omega  116.00  171.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 55

 27 omega  122.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 55

 28 omega  103.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 29 omega  110.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 68

 30 omega   80.00  107.00   1.0000    1.0000
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    -      112.0000   73.0000  -97.4918 27

 31 omega   79.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -120.0000 26

 32 omega   83.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -120.0000 67

 33 omega   84.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -30.0000 41

 34 omega   85.00  125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   30.0000 40

 35 omega   84.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   60.0000 25

 36 omega   79.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 42

 37 omega   83.00  109.00   1.0000    1.0000
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    -      112.0000   61.0000  150.0000 26

 38 omega   83.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  120.0000 93

 39 omega   84.00  174.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000    0.0000 90

 40 omega   83.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -150.0000 26

 41 omega   84.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   57.0000 -169.8742 31

 42 omega   79.00  162.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -150.0000 83

 43 omega   83.00  153.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -60.0000 70

 44 omega   83.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 45 omega   80.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   75.0000  -29.6161 26

 46 omega   79.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -60.0000 27

 47 omega   79.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 27

 48 omega   79.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 26

 49 omega   81.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   71.0000    1.4818 27

 50 omega   79.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   60.0000 27

 51 omega   79.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 26

 52 omega   79.00  105.00   1.0000    1.0000
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    -      112.0000   77.0000  120.0000 26

 53 omega   79.00  168.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  150.0000 89

 54 omega   12.00   38.00   1.0000    1.0000
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 55 omega -116.00  -87.00   1.0000    1.0000
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 56 omega -118.00  -10.00   1.0000    1.0000
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    -      -42.6216  -77.0000 -180.0000 108

 57 omega -119.00  -91.00   1.0000    1.0000
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 58 omega -119.00  -70.00   1.0000    1.0000
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 59 omega -119.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -77.0000   90.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_UB_11      0.0414195000
_diffrn_orient_matrix_UB_12      0.0783253000
_diffrn_orient_matrix_UB_13      -0.0535743000
_diffrn_orient_matrix_UB_21      0.1622045000
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_diffrn_orient_matrix_UB_23      0.0710075000
_diffrn_orient_matrix_UB_31      0.0860177000
_diffrn_orient_matrix_UB_32      -0.0559703000
_diffrn_orient_matrix_UB_33      -0.0625328000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.277
_diffrn_reflns_theta_min         4.176
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    43.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_preparation
'Reaction of lead diiodide with dipyridophenazine'
_exptl_crystal_recrystallization_method
'Crystallised from N-methyl-2- pyrrolidone and methanol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.633
_refine_diff_density_min         -3.246
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1970
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0750P)^2^+28.1990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1837
_reflns_number_total             1970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02749_si_004.cif
_cod_data_source_block           xstr0395
_cod_database_code               4347119
_chemical_oxdiff_formula         'Pb I2 C18 H10 N4'
_chemical_oxdiff_usercomment     'CEK WLT 100 K'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Sof: I2(0.5) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C8(0.5) H8(0.5) C7(0.5)
 C4(0.5) C3(0.5) H3(0.5) C2(0.5) H2(0.5) C1(0.5) H1(0.5) N1(0.5) N2(0.5)
 C6(0.5) C5(0.5) C18(0.5) H18(0.5) C17(0.5) H17(0.5) C16(0.5) H16(0.5) C15(0.5)
 H15(0.5) C14(0.5) N3(0.5) C12(0.5) C11(0.5) N4(0.5) C13(0.5) I1(0.5)
 Fixed U12: Pb1(0)
 Fixed U23: Pb1(0)
 Fixed Uiso: H10(0.039) H9(0.033) H8(0.029) H3(0.029) H2(0.033) H1(0.039)
 H18(0.041) H17(0.036) H16(0.036) H15(0.041)
 Fixed X: Pb1(0.75) H10(0.5702) H9(0.4958) H8(0.5505) H3(0.9203) H2(0.9945)
 H1(0.94) H18(0.6104) H17(0.6677) H16(0.7912) H15(0.8564)
 Fixed Y: H10(0.1243) H9(0.249) H8(0.3787) H3(0.3929) H2(0.2682) H1(0.1385)
 H18(0.6348) H17(0.7629) H16(0.7682) H15(0.6454)
 Fixed Z: Pb1(0.5) H10(0.6928) H9(0.7582) H8(0.6957) H3(0.3286) H2(0.2631)
 H1(0.3256) H18(0.656) H17(0.5936) H16(0.4597) H15(0.3894)
;
_shelx_res_checksum              73990
_shelx_hkl_checksum              13979
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-11
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_olex2_submission_original_sample_id XSTR0395
_olex2_submission_special_instructions 'No special instructions were received'