Synthesis, Properties, and Theoretical Studies of New Stepwise Layered Iodoplumbate: [Ni(opd)2(acn)2]n[Pb4I10]n
Jin-Peng Li; Long-Hua Li; Li-Ming Wu; Ling Chen; Inorganic Chemistry 48 (2009) 1260–1262; doi:10.1021/ic8012624

data_4301416
_publ_contact_author_address
;
State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian
350002
P. R. China
;
_publ_contact_author_email       chenl@fjirsm.ac.cn
_publ_contact_author_fax         (011)86-591-83704947
_publ_contact_author_name        'Ling Chen'
_publ_contact_author_phone       (011)86-591-83704947
_publ_section_title
;
Synthesis, Properties, and Theoretical Studies of New Stepwise Layered
Iodoplumbate: [Ni(opd)2(acn)2]n[Pb4I10]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1260
_journal_page_last               1262
_journal_paper_doi               10.1021/ic8012624
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C16 H22 I10 N6 Ni Pb4'
_chemical_formula_weight         2454.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.303(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9805(15)
_cell_length_b                   7.8875(7)
_cell_length_c                   19.746(2)
_cell_measurement_reflns_used    4140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.0717
_cell_volume                     2168.1(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16461
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    23.042
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2945
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    3.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.0600
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                3653
_reflns_number_total             4952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8012624_si_002.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2168.0(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4301416