Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
Imran, Muhammad; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Monkowius, Uwe; Gründlinger, Petra; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 924–937; doi:10.1039/c4dt01406e

data_7031674
_publ_section_title
;
 Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              924
_journal_page_last               937
_journal_paper_doi               10.1039/c4dt01406e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C64 H60 N20 O12 Pb2 S8, 2(C4 H8 O), 2(H2 O)'
_chemical_formula_sum            'C72 H80 N20 O16 Pb2 S8'
_chemical_formula_weight         2152.42
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0600(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8252(2)
_cell_length_b                   20.7570(2)
_cell_length_c                   15.8960(2)
_cell_measurement_reflns_used    94289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     8521.10(15)
_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24540
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.155
_exptl_absorpt_coefficient_mu    4.218
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.690436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.774
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0359P)^2^+22.5869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9591
_reflns_number_total             12428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7031671--7031680.cif.'
_cod_database_code               7031674
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.407
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O8A, O8B}
{C34A, C34B}
3. Restrained distances
 C33A-C34A \\sim C34A-C35A
 with sigma of 0.02
 C33B-C34B \\sim C34B-C35B
 with sigma of 0.02
 C16-C13 \\sim C16B-C14
 with sigma of 0.02
 C24B-C21 \\sim C24-C22
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O8A) = Uanis(O8B)
Uanis(C34A) = Uanis(C34B)
5. Same fragment restrains
{O8A, C36A, C35A, C34A, C33A}
as
{O8A, C33A, C34A, C35A, C36A}
{O8B, C36B, C35B, C34B, C33B}
as
{O8B, C33B, C34B, C35B, C36B}
6. Others
 Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
 Sof(O8B)=Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=
 Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=1-FVAR(3)
 Sof(O8A)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C33A(H33A,H33B), C34A(H34A,H34B), C35A(H35A,H35B), C36A(H36A,H36B), C33B(H33C,
 H33D), C34B(H34C,H34D), C35B(H35C,H35D), C36B(H36C,H36D)
7.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), C4(H4A),
 C5(H5A), C7(H7A), C12(H12), C15(H15), C20(H20), C23(H23), C28(H28), C29(H29),
 C31(H31)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C24(H24A,H24B,
 H24C), C24B(H24D,H24E,H24F), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              43439
_olex2_submission_special_instructions 'No special instructions were received'