Catalytically active lead(ii)-imidazolium coordination assemblies with diversified lead(ii) coordination geometries.
Naga Babu, Chatla; Suresh, Paladugu; Srinivas, Katam; Sathyanarayana, Arruri; Sampath, Natarajan; Prabusankar, Ganesan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8164–8173; doi:10.1039/c5dt04409j

data_7038927
_publ_section_title
;
 Catalytically active lead(ii)-imidazolium coordination assemblies with
 diversified lead(ii) coordination geometries.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8164
_journal_page_last               8173
_journal_paper_doi               10.1039/c5dt04409j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C84 H64 Br4.75 Cl2.27 N18 O21.25 Pb6, 12.2(O), 0.5(N O3)'
_chemical_formula_sum            'C84 H64 Br4.74 Cl2.29 N18.5 O34.95 Pb6'
_chemical_formula_weight         3594.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-29
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6333(7)
_cell_length_b                   19.2972(5)
_cell_length_c                   19.7693(5)
_cell_measurement_reflns_used    11652
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.883
_cell_measurement_theta_min      3.200
_cell_volume                     12067.9(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_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    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33506
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.883
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.905
_exptl_absorpt_correction_T_max  01235
_exptl_absorpt_correction_T_min  0.0351
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
C.W.Dwiggins Jr Acta Cryst.(1975) A31,146-148) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       Block
_exptl_crystal_F_000             6695
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.1400
_refine_diff_density_max         2.539
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         11802
_refine_ls_number_restraints     814
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8728
_reflns_number_total             11802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04409j3.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Sphere' changed to 'sphere'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7038926--7038930.cif.
;
_cod_original_formula_sum        'C84 H64 Br4.74 Cl2.29 N18.50 O34.95 Pb6'
_cod_database_code               7038927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Br6, Cl3}
{Br4, Cl4}
{Br5, Cl5}
{Br2, Cl2}
{Br1, Cl1}
{Br3, Cl6}
3. Restrained distances
 O9-O11
 2.2 with sigma of 0.02
 O5-N13 \\sim O3-N13 \\sim O2-N13
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Br6) = Uanis(Cl3)
Uanis(Br4) = Uanis(Cl4)
Uanis(Br5) = Uanis(Cl5)
Uanis(Br1) = Uanis(Cl1)
Uanis(Br2) = Uanis(Cl2)
Uanis(Br3) = Uanis(Cl6)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl1)=0.5*(1-FVAR(2))
 Sof(Br1)=0.5*FVAR(2)
 Fixed Sof: Br2(0.415) Br3(0.325) Br4(0.25) Br5(0.8) Br6(0.255) Cl2(0.085)
 Cl3(0.18) Cl4(0.25) Cl5(0.2) Cl6(0.25) O11(0.125) O16(0.6) O20(0.35) O23(0.5)
 O27(0.15) O2(0.25) O3(0.25) O5(0.25) N13(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C33(H33A,H33B), C44(H44A,H44B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43)
;
_shelx_res_checksum              78292
_shelx_shelxl_version_number     2014/8
_olex2_submission_special_instructions 'No special instructions were received'