#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:11:53 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179618 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/82/4508242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4508242
loop_
_publ_author_name
'Mukherjee, Gargi'
'Biradha, Kumar'
_publ_section_title
;
 Coordination Polymers Containing M2L2and M4L4Metallacylces of
 Bis(pyridylcarboxamido)alkanes with an Odd Number of −(CH2)--
 Groups as Spacers: Guest Inclusion and Networks Recognition via α Sheet
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4100
_journal_paper_doi               10.1021/cg400918d
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C30 H32 Cu4 I4 N8 O4'
_chemical_formula_weight         1330.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.489(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.158(4)
_cell_length_b                   10.0274(14)
_cell_length_c                   15.632(2)
_cell_measurement_reflns_used    3589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.58
_cell_volume                     4031.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-2 CCD'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22321
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    5.188
_exptl_absorpt_correction_T_max  0.459
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.755
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.593
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.593
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0732
_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/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2102
_reflns_number_gt                3080
_reflns_number_total             3589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400918d_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4031.9(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4508242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.58633(3) -0.14618(7) -0.15844(5) 0.0509(3) Uani 1 1 d .
I2 I 0.53912(3) -0.42800(7) -0.37606(5) 0.0534(3) Uani 1 1 d .
Cu2 Cu 0.54837(6) -0.38621(16) -0.20785(10) 0.0595(5) Uani 1 1 d .
Cu1 Cu 0.51240(6) -0.19467(15) -0.32960(13) 0.0667(5) Uani 1 1 d .
O16 O 0.6850(4) -0.4393(7) 0.0886(7) 0.073(3) Uani 1 1 d .
N11 N 0.5966(4) -0.5306(10) -0.1470(6) 0.050(2) Uani 1 1 d .
C11 C 0.6552(4) -0.6002(10) -0.0154(7) 0.043(2) Uani 1 1 d .
C12 C 0.6230(4) -0.5088(11) -0.0676(7) 0.045(2) Uani 1 1 d .
H12 H 0.6198 -0.4246 -0.0442 0.054 Uiso 1 1 calc R
C13 C 0.6006(7) -0.6529(12) -0.1810(10) 0.071(4) Uani 1 1 d .
H13 H 0.5834 -0.6708 -0.2372 0.085 Uiso 1 1 calc R
C14 C 0.6295(7) -0.7505(12) -0.1348(10) 0.078(5) Uani 1 1 d .
H14 H 0.6298 -0.8354 -0.1586 0.094 Uiso 1 1 calc R
C15 C 0.6580(6) -0.7261(12) -0.0537(9) 0.070(4) Uani 1 1 d .
H15 H 0.6791 -0.7924 -0.0242 0.084 Uiso 1 1 calc R
C16 C 0.6819(4) -0.5582(10) 0.0713(8) 0.044(2) Uani 1 1 d .
O26 O 0.7991(3) -0.4414(7) 0.3908(6) 0.058(2) Uani 1 1 d .
N21 N 0.9554(4) -0.4603(9) 0.3826(6) 0.049(2) Uani 1 1 d .
C21 C 0.8772(4) -0.5691(9) 0.3984(6) 0.039(2) Uani 1 1 d .
C22 C 0.9037(4) -0.4576(10) 0.3839(7) 0.046(3) Uani 1 1 d .
H22 H 0.8859 -0.3770 0.3745 0.056 Uiso 1 1 calc R
C23 C 0.9805(5) -0.5756(10) 0.4007(8) 0.050(3) Uani 1 1 d .
H23 H 1.0162 -0.5780 0.4016 0.060 Uiso 1 1 calc R
C24 C 0.9563(5) -0.6892(11) 0.4179(8) 0.055(3) Uani 1 1 d .
H24 H 0.9754 -0.7674 0.4301 0.066 Uiso 1 1 calc R
C25 C 0.9025(4) -0.6893(11) 0.4175(8) 0.052(3) Uani 1 1 d .
H25 H 0.8849 -0.7658 0.4294 0.062 Uiso 1 1 calc R
C26 C 0.8195(4) -0.5541(10) 0.3950(7) 0.044(2) Uani 1 1 d .
N31 N 0.7909(4) -0.6640(9) 0.3906(6) 0.048(2) Uani 1 1 d .
H31 H 0.8065 -0.7398 0.3981 0.057 Uiso 1 1 calc R
N32 N 0.7031(4) -0.6495(10) 0.1259(7) 0.057(3) Uani 1 1 d .
H32 H 0.7013 -0.7314 0.1093 0.068 Uiso 1 1 calc R
C31 C 0.7332(5) -0.6614(13) 0.3734(10) 0.066(4) Uani 1 1 d .
H31A H 0.7212 -0.5721 0.3829 0.079 Uiso 1 1 calc .
H31B H 0.7202 -0.7212 0.4133 0.079 Uiso 1 1 calc .
C32 C 0.7118(5) -0.7042(14) 0.2796(9) 0.064(3) Uani 1 1 d .
H32A H 0.7224 -0.7954 0.2718 0.076 Uiso 1 1 calc .
H32B H 0.6742 -0.7025 0.2702 0.076 Uiso 1 1 calc .
C33 C 0.7295(5) -0.6191(13) 0.2130(8) 0.065(4) Uani 1 1 d .
H33A H 0.7235 -0.5263 0.2256 0.078 Uiso 1 1 calc .
H33B H 0.7666 -0.6312 0.2163 0.078 Uiso 1 1 calc .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cu1 I1 Cu2 59.83(5) 2_654 .
Cu1 I1 Cu1 56.14(7) 2_654 .
Cu2 I1 Cu1 57.10(4) . .
Cu1 I2 Cu2 63.58(6) . .
Cu1 I2 Cu2 57.31(5) . 2_654
Cu2 I2 Cu2 57.00(5) . 2_654
N11 Cu2 I2 106.8(3) . .
N11 Cu2 Cu1 139.8(3) . 2_654
I2 Cu2 Cu1 112.96(7) . 2_654
N11 Cu2 Cu2 133.7(3) . 2_654
I2 Cu2 Cu2 66.06(6) . 2_654
Cu1 Cu2 Cu2 62.99(6) 2_654 2_654
N11 Cu2 I1 109.9(3) . .
I2 Cu2 I1 113.29(7) . .
Cu1 Cu2 I1 58.89(5) 2_654 .
Cu2 Cu2 I1 114.76(3) 2_654 .
N11 Cu2 Cu1 157.6(3) . .
I2 Cu2 Cu1 57.39(5) . .
Cu1 Cu2 Cu1 59.88(9) 2_654 .
Cu2 Cu2 Cu1 58.41(5) 2_654 .
I1 Cu2 Cu1 68.39(6) . .
N11 Cu2 I2 99.2(3) . 2_654
I2 Cu2 I2 119.88(6) . 2_654
Cu1 Cu2 I2 55.89(5) 2_654 2_654
Cu2 Cu2 I2 56.94(7) 2_654 2_654
I1 Cu2 I2 106.60(6) . 2_654
Cu1 Cu2 I2 102.58(6) . 2_654
N21 Cu1 I2 115.3(3) 7_645 .
N21 Cu1 I1 108.1(3) 7_645 2_654
I2 Cu1 I1 117.71(7) . 2_654
N21 Cu1 Cu2 166.0(3) 7_645 2_654
I2 Cu1 Cu2 66.80(6) . 2_654
I1 Cu1 Cu2 61.28(5) 2_654 2_654
N21 Cu1 Cu1 124.8(3) 7_645 2_654
I2 Cu1 Cu1 112.59(5) . 2_654
I1 Cu1 Cu1 70.26(6) 2_654 2_654
Cu2 Cu1 Cu1 62.29(6) 2_654 2_654
N21 Cu1 Cu2 135.0(3) 7_645 .
I2 Cu1 Cu2 59.03(5) . .
I1 Cu1 Cu2 113.01(7) 2_654 .
Cu2 Cu1 Cu2 58.60(7) 2_654 .
Cu1 Cu1 Cu2 57.83(6) 2_654 .
N21 Cu1 I1 89.5(3) 7_645 .
I2 Cu1 I1 103.34(6) . .
I1 Cu1 I1 119.82(7) 2_654 .
Cu2 Cu1 I1 103.56(7) 2_654 .
Cu1 Cu1 I1 53.60(7) 2_654 .
Cu2 Cu1 I1 54.51(5) . .
C12 N11 C13 117.0(10) . .
C12 N11 Cu2 119.5(7) . .
C13 N11 Cu2 123.3(8) . .
C15 C11 C12 114.3(10) . .
C15 C11 C16 126.7(10) . .
C12 C11 C16 119.0(9) . .
N11 C12 C11 126.4(10) . .
N11 C13 C14 121.5(13) . .
C15 C14 C13 121.2(12) . .
C14 C15 C11 119.5(11) . .
O16 C16 N32 122.4(11) . .
O16 C16 C11 119.0(10) . .
N32 C16 C11 118.5(9) . .
C23 N21 C22 118.0(9) . .
C23 N21 Cu1 121.9(8) . 7_645
C22 N21 Cu1 118.8(7) . 7_645
C22 C21 C25 121.1(11) . .
C22 C21 C26 116.8(9) . .
C25 C21 C26 122.1(9) . .
C21 C22 N21 121.8(10) . .
C24 C23 N21 122.7(11) . .
C23 C24 C25 120.2(10) . .
C21 C25 C24 116.1(10) . .
O26 C26 N31 121.3(11) . .
O26 C26 C21 120.6(9) . .
N31 C26 C21 118.0(10) . .
C26 N31 C31 122.7(10) . .
C16 N32 C33 122.9(11) . .
N31 C31 C32 110.5(10) . .
C33 C32 C31 113.9(10) . .
N32 C33 C32 112.6(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.6009(17) 2_654
I1 Cu2 2.6639(17) .
I1 Cu1 3.042(2) .
I2 Cu1 2.5836(18) .
I2 Cu2 2.6300(18) .
I2 Cu2 2.868(2) 2_654
Cu2 N11 2.038(9) .
Cu2 Cu1 2.626(2) 2_654
Cu2 Cu2 2.632(3) 2_654
Cu2 Cu1 2.747(2) .
Cu2 I2 2.868(2) 2_654
Cu1 N21 2.017(9) 7_645
Cu1 I1 2.6009(17) 2_654
Cu1 Cu2 2.626(2) 2_654
Cu1 Cu1 2.684(4) 2_654
O16 C16 1.223(12) .
N11 C12 1.325(14) .
N11 C13 1.348(16) .
C11 C15 1.405(16) .
C11 C12 1.402(14) .
C11 C16 1.467(15) .
C13 C14 1.361(18) .
C14 C15 1.372(19) .
C16 N32 1.305(14) .
O26 C26 1.247(13) .
N21 C23 1.335(14) .
N21 C22 1.356(15) .
N21 Cu1 2.017(9) 7_645
C21 C22 1.356(14) .
C21 C25 1.382(14) .
C21 C26 1.507(16) .
C23 C24 1.353(16) .
C24 C25 1.408(17) .
C26 N31 1.326(13) .
N31 C31 1.487(16) .
N32 C33 1.442(15) .
C31 C32 1.53(2) .
C32 C33 1.483(19) .
