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_7209678
_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         'C38 H24 Cu2 I4 N2 O8'
_chemical_formula_sum            'C38 H24 Cu2 I4 N2 O8'
_chemical_formula_weight         1271.27
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.821(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.230(3)
_cell_length_b                   22.664(5)
_cell_length_c                   27.692(5)
_cell_measurement_reflns_used    1558
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      16.848
_cell_measurement_theta_min      2.435
_cell_volume                     9320(3)
_computing_data_reduction        'SAINT v6.45A (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      150.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1888
_diffrn_reflns_av_unetI/netI     0.3486
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25328
_diffrn_reflns_theta_full        21.05
_diffrn_reflns_theta_max         21.05
_diffrn_reflns_theta_min         0.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.608
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.056012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0885 before and 0.0558 after correction.
The Ratio of minimum to maximum transmission is 0.056012.
The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.891
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         10006
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.3100
_refine_ls_R_factor_gt           0.1425
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3537
_refine_ls_wR_factor_ref         0.4112
_reflns_number_gt                2769
_reflns_number_total             10006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce26919a.txt
_cod_data_source_block           ilb1173_0m
_cod_database_code               7209678
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H82 of C82, H2 of C2, H16 of C16, H88 of C88, H93 of C93, H95 of C95, H9C
of C9C, H99 of C99, H22 of C22, H92 of C92, H89 of C89, H73 of C73, H86 of
C86, H66 of C66, H72 of C72, H3 of C3, H25 of C25, H65 of C65, H56 of C56, H6
of C6, H12 of C12, H96 of C96, H13 of C13, H46 of C46, H45 of C45, H23 of C23,
H32 of C32, H8C of C8C, H98 of C98, H33 of C33, H55 of C55, H76 of C76, H63
of C63, H5 of C5, H75 of C75, H52 of C52, H62 of C62, H85 of C85, H36 of C36,
H42 of C42, H8B of C8B, H9B of C9B, H53 of C53, H15 of C15, H35 of C35, H43
of C43, H83 of C83, H26 of C26
2. Restrained distances
C64-I64A ~ C64-I64B
with sigma of 0.0001
3. Rigid bond restraints
C11, C12, C13, C14, C15, C16
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C82, C83, C84, C85, C86
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C61, C62, C64, C65, C66, C63
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C54, C55, C56, C51, C52, C53
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13 ~ C12 ~ C14 ~ C15 ~ C16 ~ C11: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C86 ~ C85 ~ N81 ~ C82 ~ C83 ~ C84: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C66 ~ C61 ~ C62 ~ C63 ~ C64 ~ C65: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C53 ~ C52 ~ C51 ~ C56 ~ C55 ~ C54: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(I4B) = Uanis(I4A)
Uanis(I64A) = Uanis(I64B)
5. Others
Sof(I4A)=1-Sof(I4B)
Sof(I64A)=1-Sof(I64B)
6.a Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C15(H15), C16(H16),
C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C36(H36), C35(H35),
C42(H42), C43(H43), C45(H45), C46(H46), C52(H52), C53(H53), C55(H55),
C56(H56), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75),
C76(H76), C82(H82), C83(H83), C85(H85), C86(H86), C92(H92), C93(H93),
C95(H95), C96(H96), C88(H88), C89(H89), C8B(H8B), C8C(H8C), C98(H98), C99(H99),
C9B(H9B), C9C(H9C)
6.b Fitted hexagon refined as free rotating group:
C1(C2,C3,C4,C5,C6), C11(C12,C13,C14,C15,C16), C21(C22,C23,C24,C25,C26),
C31(C32,C33,C34,C36,C35), C41(C42,C43,C44,C45,C46), C51(C52,C53,C54,C55,C56),
C61(C62,C63,C64,C65,C66), C71(C72,C73,C74,C75,C76), N81(C82,C83,C84,C85,C86),
N91(C92,C93,C94,C95,C96), N87(C88,C89,C8A,C8B,C8C), N97(C98,C99,C9A,C9B,C9C)
;