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_7209679
_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         'C52 H40 Cu2 I4 N4 O8, 2(C7 H8 O)'
_chemical_formula_sum            'C66 H56 Cu2 I4 N4 O10'
_chemical_formula_weight         1699.83
_chemical_name_systematic
;
?
;
_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                102.764(17)
_cell_angle_beta                 98.004(16)
_cell_angle_gamma                101.353(14)
_cell_formula_units_Z            2
_cell_length_a                   8.2079(19)
_cell_length_b                   16.029(4)
_cell_length_c                   24.699(6)
_cell_measurement_reflns_used    323
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.68
_cell_volume                     3049.9(13)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_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     0.1972
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15917
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         0.86
_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    2.785
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.421601
_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 0.1410 before and 0.0953 after correction.
The Ratio of minimum to maximum transmission not present.
The \l/2 correction factor is Not present
For component 2:
wR2(int) was 0.1419 before and 0.0989 after correction.
The Ratio of minimum to maximum transmission is 0.57.
The \l/2 correction factor is Not present
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.479
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         15920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.2310
_refine_ls_R_factor_gt           0.1080
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2654
_refine_ls_wR_factor_ref         0.3417
_reflns_number_gt                6714
_reflns_number_total             15920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce26919a.txt
_cod_data_source_block           twin4_a
_cod_original_cell_volume        3049.9(12)
_cod_database_code               7209679
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H62 of C62, H32 of C32, {H59a,H59b} of C59, H11 of C11, H35 of C35, H39 of
C39, H25 of C25, H12 of C12, H40 of C40, H53 of C53, H42 of C42, H61 of C61,
H3 of C3, H64 of C64, H60 of C60, H4 of C4, H14 of C14, H18 of C18, H52 of
C52, {H6a,H6b} of C6, H21 of C21, H13 of C13, H20 of C20, H26 of C26, H5 of
C5, H28 of C28, H36 of C36, H54 of C54, H49 of C49, H65 of C65, {H57a,H57b}
of C57, H9 of C9, H16 of C16, H43 of C43, H47 of C47, H27 of C27, H46 of C46,
H1 of C1, H10 of C10, H17 of C17, H55 of C55, H50 of C50, {H58a,H58b} of C58,
H19 of C19, {H66a,H66b} of C66, H56 of C56, H33 of C33, {H7a,H7b} of C7
At 1.5 times of:
H10a of O10, H9a of O9
2.a Secondary CH2 refined with riding coordinates:
C7(H7a,H7b), C6(H6a,H6b), C57(H57a,H57b), C58(H58a,H58b), C66(H66a,H66b),
C59(H59a,H59b)
2.b Aromatic/amide H refined with riding coordinates:
C36(H36), C18(H18), C33(H33), C17(H17), C1(H1), C56(H56), C49(H49), C43(H43),
C26(H26), C40(H40), C4(H4), C9(H9), C25(H25), C16(H16), C50(H50), C12(H12),
C13(H13), C53(H53), C21(H21), C46(H46), C20(H20), C47(H47), C52(H52), C28(H28),
C14(H14), C11(H11), C32(H32), C3(H3), C27(H27), C42(H42), C39(H39), C35(H35),
C5(H5), C10(H10), C54(H54), C55(H55), C19(H19), C62(H62), C64(H64), C65(H65),
C60(H60), C61(H61)
2.c Idealised tetrahedral OH refined as rotating group:
O9(H9a), O10(H10a)
;