Persistent C–I⋯π halogen-bonded layer motifs involving 4-iodobenzoate paddlewheel units, Cu2(4-Ibz)4(L)2
Smart, Paul; Bejarano-Villafuerte, Ángela; Hendry, Rebecca M.; Brammer, Lee; CrystEngComm 15 (2013) 3160–; doi:10.1039/c3ce26919a

data_7209674
_publ_section_title
;
 Persistent C--I&#x22EF;\p halogen-bonded layer motifs involving
 4-iodobenzoate paddlewheel units, Cu2(4-Ibz)4(L)2
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              3160
_journal_paper_doi               10.1039/c3ce26919a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C32 H28 Cu2 I4 O10 S2'
_chemical_formula_sum            'C32 H28 Cu2 I4 O10 S2'
_chemical_formula_weight         1271.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-07
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                92.436(6)
_cell_angle_beta                 90.283(6)
_cell_angle_gamma                93.469(6)
_cell_formula_units_Z            2
_cell_length_a                   6.5847(5)
_cell_length_b                   15.8533(13)
_cell_length_c                   18.2578(15)
_cell_measurement_reflns_used    2665
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.282
_cell_measurement_theta_min      2.58
_cell_volume                     1900.7(3)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8615
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
For component 1:
wR2(int) was 0.0765 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.70.
The \l/2 correction factor is Not present
For component 2:
wR2(int) was 0.1212 before and 0.0831 after correction.
The Ratio of minimum to maximum transmission is 0.70.
The \l/2 correction factor is Not present
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.516
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8615
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                5951
_reflns_number_total             8615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce26919a.txt
_cod_data_source_block           twin4
_cod_database_code               7209674
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H17 of C17, H20 of C20, H11 of C11, H28 of C28, H13 of C13, H4 of C4, H24
of C24, H10 of C10, H3 of C3, H27 of C27, H25 of C25, H21 of C21, H6 of C6,
H14 of C14, H7 of C7, H18 of C18
At 1.5 times of:
{H30a,H30b,H30c} of C30, {H32a,H32b,H32c} of C32, {H29a,H29b,H29c} of C29,
{H31a,H31b,H31c} of C31
2. Uiso/Uaniso restraints and constraints
Uanis(C1) ~ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) ~ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
C24(H24), C17(H17), C6(H6), C14(H14), C10(H10), C13(H13), C3(H3), C4(H4),
C21(H21), C28(H28), C7(H7), C18(H18), C20(H20), C25(H25), C27(H27), C11(H11)
3.b Idealised Me refined as rotating group:
C30(H30a,H30b,H30c), C29(H29a,H29b,H29c), C31(H31a,H31b,H31c), C32(H32a,H32b,
H32c)
;