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_4347118
_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         'C44 H24 I2 N8 Pb'
_chemical_formula_sum            'C44 H24 I2 N8 Pb'
_chemical_formula_weight         1125.70
_chemical_name_systematic        PbI2dppn
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_beta                 91.8576(14)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   26.1924(4)
_cell_length_b                   12.5713(2)
_cell_length_c                   33.1849(5)
_cell_measurement_reflns_used    12392
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.5830
_cell_measurement_theta_min      4.7050
_cell_volume                     10921.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega -116.00  -48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6216  -57.0000 -180.0000 68

  2 omega  -79.00   26.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6216   19.0000 -180.0000 105

  3 omega  109.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614  125.0000  -60.0000 69

  4 omega   78.00  172.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614   30.0000    0.0000 94

  5 omega   84.00  178.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614   30.0000   90.0000 94

  6 omega   29.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3614  -94.0000 -120.0000 80

  7 omega  -95.00   -7.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8716  125.0000    0.0000 88

  8 omega  -47.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.8716   38.0000  -90.0000 57

  9 omega   42.00   85.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8716 -121.0000  176.0000 43

 10 omega    1.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8716  -99.0000  -30.0000 59

 11 omega   39.00   65.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 26

 12 omega   85.00  111.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 26

 13 omega   37.00   91.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 54

 14 omega   84.00  115.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 31

 15 omega   46.00  140.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000  -90.0000 94

 16 omega  120.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000   60.0000 57

 17 omega   36.00   85.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 49

 18 omega  100.00  126.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 26

 19 omega  130.00  170.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 40

 20 omega   37.00   63.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -180.0000 26

 21 omega   86.00  100.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000    0.0000 14
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0293394000
_diffrn_orient_matrix_UB_12      -0.0413700000
_diffrn_orient_matrix_UB_13      -0.0363240000
_diffrn_orient_matrix_UB_21      -0.0450067000
_diffrn_orient_matrix_UB_22      0.0322431000
_diffrn_orient_matrix_UB_23      -0.0284597000
_diffrn_orient_matrix_UB_31      0.0240210000
_diffrn_orient_matrix_UB_32      0.1107586000
_diffrn_orient_matrix_UB_33      -0.0052629000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.696
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       plate
_exptl_crystal_F_000             6384
_exptl_crystal_preparation
'dppn and lead (II) iodide were separately dissolved in minimum amounts of NMP and layered.'
_exptl_crystal_recrystallization_method 'Layered in NMP'
_exptl_crystal_size_max          0.0658
_exptl_crystal_size_mid          0.0323
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0418P)^2^+71.0727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8882
_reflns_number_total             11082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02749_si_002.cif
_cod_data_source_block           xstr0409
_cod_database_code               4347118
_chemical_oxdiff_formula         'Pb I2 C44 N8 H24'
_chemical_oxdiff_usercomment     'Very thin crystal'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I1D) = Uanis(I2D)
Uanis(I1D) = Uanis(I3D)
3. Others
 Sof(I1D)=Sof(I2D)=Sof(Pb1D)=Sof(I3D)=1-FVAR(1)
 Sof(Pb2D)=0.5*(1-FVAR(2))
 Sof(Pb2)=0.5*FVAR(2)
 Sof(I1)=Sof(I2)=Sof(Pb1)=Sof(I3)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C1A(H1A), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C8A(H8A),
 C8B(H8B), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B), C14A(H14A), C14B(H14B),
 C17A(H17A), C17B(H17B), C19A(H19A), C19B(H19B), C20A(H20A), C20B(H20B),
 C21A(H21A), C21B(H21B), C22A(H22A), C22B(H22B), C1C(H1C), C2C(H2C), C3C(H3C),
 C8C(H8C), C9C(H9C), C10C(H10C), C14C(H14C), C17C(H17C), C19C(H19C), C20C(H20C),
  C21C(H21C), C22C(H22C)
;
_shelx_res_checksum              37677
_shelx_hkl_checksum              76038
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-30
_olex2_exptl_crystal_mounting_method 'Mounted on a nylon loop'
_olex2_submission_original_sample_id XSTR0409
_olex2_submission_special_instructions 'No special instructions were received'
_usercomment
'Ligands are labelled with the subsection A B and C to indicate the three different ligand environments in the asymmetric unit'