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_7209676
_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         'C34 H30 Cu2 I4 N2 O10, 4(C3 H7 N O)'
_chemical_formula_sum            'C46 H58 Cu2 I4 N6 O14'
_chemical_formula_weight         1553.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 96.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.997(3)
_cell_length_b                   12.621(3)
_cell_length_c                   16.880(3)
_cell_measurement_reflns_used    1759
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.42
_cell_volume                     2753.0(10)
_computing_data_reduction        'SAINT v7.23A (Bruker, 2003)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.929
_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     0.0437
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18555
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.88
_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    3.082
_exptl_absorpt_correction_T_max  0.746072
_exptl_absorpt_correction_T_min  0.544531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_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    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         18635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+1.1203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                15548
_reflns_number_total             18635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce26919a.txt
_cod_data_source_block           hkl5
_cod_database_code               7209676
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H16 of C16, H1S of C1S, H5 of C5, H2 of C2, H3 of C3, {H3SA,H3SB,H3SC} of
C3S, H11S of C11S, {H22A,H22B,H22C} of C22S, H15 of C15, H21S of C21S, H12 of
C12, {H2SA,H2SB,H2SC} of C2S, H6 of C6, H13 of C13, {H23A,H23B,H23C} of C23S
At 1.5 times of:
{H12D,H12E,H12F} of C12T, {H13D,H13E,H13F} of C13T, {H13A,H13B,H13C} of
C13S, {H12A,H12B,H12C} of C12S
2. Uiso/Uaniso restraints and constraints
Uanis(C13S) = Uanis(C13T)
Uanis(C12S) = Uanis(C12T)
3. Others
Sof(C12S)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13S)=Sof(H13A)=Sof(H13B)=
Sof(H13C)=1-Sof(H12A)=1-Sof(H12A)=1-Sof(H12A)=1-Sof(H12A)=1-Sof(H12A)=1-
Sof(H12A)=1-Sof(H12A)=1-Sof(H12A)
4.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
C1S(H1S), C11S(H11S), C21S(H21S)
4.b Idealised Me refined as rotating group:
C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C12S(H12A,H12B,H12C), C13S(H13A,
H13B,H13C), C22S(H22A,H22B,H22C), C23S(H23A,H23B,H23C), C13T(H13D,H13E,H13F),
C12T(H12D,H12E,H12F)
;