Crystal structures and photocatalytic properties of two novel iodoplumbate hybrids templated by multivalent organic cations
Wang, Chao-Hai; Du, Hai-Juan; Li, Yao; Niu, Yun-Yin; Hou, Hong-Wei; New J. Chem. 39 (2015) 7372–; doi:10.1039/C5NJ01240F

data_7055003
_publ_section_title
;
 Crystal structures and photocatalytic properties of two novel
 iodoplumbate hybrids templated by multivalent organic cations
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7372
_journal_paper_doi               10.1039/C5NJ01240F
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C27 H30 N3, I9 Pb3, O'
_chemical_formula_sum            'C27 H32 I9 N3 O Pb3'
_chemical_formula_weight         2178.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-07 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.571(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5741(6)
_cell_length_b                   15.1598(5)
_cell_length_c                   15.9810(7)
_cell_measurement_reflns_used    2871
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.1280
_cell_measurement_theta_min      3.4970
_cell_volume                     4700.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -17.00   12.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   90.0000 29

  2 omega   39.00   86.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000  -90.0000 47

  3 omega  -10.00   41.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -57.0000 -180.0000 51

  4 omega   -9.00   89.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   77.0000  -60.0000 98

  5 omega  -53.00  -28.00   1.0000   19.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -37.0000  -30.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0279623000
_diffrn_orient_matrix_UB_12      0.0260351000
_diffrn_orient_matrix_UB_13      0.0189074000
_diffrn_orient_matrix_UB_21      -0.0210332000
_diffrn_orient_matrix_UB_22      0.0382070000
_diffrn_orient_matrix_UB_23      -0.0053447000
_diffrn_orient_matrix_UB_31      -0.0105627000
_diffrn_orient_matrix_UB_32      -0.0071681000
_diffrn_orient_matrix_UB_33      0.0402442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10807
_diffrn_reflns_point_group_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.078
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Flack x determined using 1388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6888
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0310P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.436
_reflns_friedel_fraction_full    0.444
_reflns_friedel_fraction_max     0.436
_reflns_number_gt                5327
_reflns_number_total             6888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01240f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055002--7055003.cif.'
_cod_database_code               7055003
_audit_block_doi                 10.5517/cc14pymd
_chemical_oxdiff_formula         C20H20N4Ag1
_shelx_estimated_absorpt_t_max   0.204
_shelx_estimated_absorpt_t_min   0.154
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C9, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C2, C3, C5, C1, C23, C24, C25, C26, C22, C27, C4, C8, C16, C17, C18, C19, C20,
  C21, C6, C11, C10, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, N1, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              87734
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'