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_7209675
_publ_section_title
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 Persistent C--I&#x22EF;\p halogen-bonded layer motifs involving
 4-iodobenzoate paddlewheel units, Cu2(4-Ibz)4(L)2
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_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'
_chemical_formula_sum            'C32 H28 Cu2 I4 O10'
_chemical_formula_weight         1207.22
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-07
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                74.517(7)
_cell_angle_beta                 68.073(7)
_cell_angle_gamma                87.380(8)
_cell_formula_units_Z            2
_cell_length_a                   12.196(2)
_cell_length_b                   13.011(2)
_cell_length_c                   13.015(2)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.50
_cell_volume                     1843.0(5)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0679
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37498
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.557
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0820 after correction.
The Ratio of minimum to maximum transmission is 0.8039.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.644
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0350P)^2^+2.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                5607
_reflns_number_total             8303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce26919a.txt
_cod_data_source_block           ilb2088_0m
_cod_original_cell_volume        1842.9(5)
_cod_database_code               7209675
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H7 of C7, H14 of C14, H3 of C3, H29 of C29, H26 of C26, {H30a,H30b} of C30,
H13 of C13, H28 of C28, H17 of C17, {H32a,H32b,H32c,H32d} of C32, H4 of C4,
H21 of C21, H11 of C11, H10 of C10, H18 of C18, H20 of C20, H25 of C25, H6 of
C6
At 1.5 times of:
{H34a,H34b,H34c} of C34, H10a of O10, {H33d,H33e,H33f} of C33A, H9 of O9,
{H33a,H33b,H33c} of C33
2. Restrained distances
O9-H9
0.85 with sigma of 0.01
O10-H10a
0.85 with sigma of 0.01
C30-H9
1.884885 with sigma of 0.02
C32-H10a
1.889448 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C33A)
4. Others
Sof(H32a)=Sof(H32b)=1-Sof(H32b)=1-Sof(H32b)=Sof(C33)=Sof(H33a)=Sof(H33b)=
Sof(H33c)=1-Sof(H32b)=1-Sof(H32b)=1-Sof(H32b)=1-Sof(H32b)
5.a Secondary CH2 refined with riding coordinates:
C30(H30a,H30b), C32(H32a,H32b), C32(H32c,H32d)
5.b Aromatic/amide H refined with riding coordinates:
C14(H14), C21(H21), C6(H6), C20(H20), C3(H3), C29(H29), C7(H7), C18(H18),
C17(H17), C28(H28), C11(H11), C4(H4), C10(H10), C13(H13), C26(H26), C25(H25)
5.c Idealised Me refined as rotating group:
C34(H34a,H34b,H34c), C33(H33a,H33b,H33c), C33A(H33d,H33e,H33f)
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