#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:11:53 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179618 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/82/4508250.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_4508250
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            'C36 H45 Cl2 Cu N9 O18'
_chemical_formula_weight         1026.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.064(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.545(3)
_cell_length_b                   11.8660(15)
_cell_length_c                   16.909(2)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.84
_cell_volume                     4437.4(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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52434
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0793
_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          0.1879
_refine_ls_wR_factor_ref         0.2095
_reflns_number_gt                5031
_reflns_number_total             8113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400918d_si_002.cif
_cod_data_source_block           10
_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        4437.3(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4508250
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cu1 Cu 0.25555(3) 0.75219(5) 0.23876(4) 0.0468(2) Uani 1 1 d .
Cl1 Cl 0.02347(8) 1.34959(16) 0.64839(9) 0.0716(5) Uani 1 1 d .
O104 O 0.0212(3) 1.4038(6) 0.5752(3) 0.119(2) Uani 1 1 d .
O103 O -0.0319(4) 1.3731(8) 0.6600(6) 0.184(4) Uani 1 1 d .
O102 O 0.0642(4) 1.3828(9) 0.7185(4) 0.198(4) Uani 1 1 d .
O101 O 0.0250(6) 1.2338(7) 0.6382(6) 0.224(5) Uani 1 1 d .
Cl2 Cl 0.46917(7) 0.34842(12) 0.33057(9) 0.0585(4) Uani 1 1 d .
O201 O 0.4398(4) 0.2531(6) 0.3424(4) 0.158(3) Uani 1 1 d .
O202 O 0.4348(4) 0.3984(7) 0.2583(4) 0.178(3) Uani 1 1 d .
O203 O 0.4823(4) 0.4141(6) 0.4007(4) 0.152(3) Uani 1 1 d .
O204 O 0.5224(3) 0.3233(7) 0.3163(5) 0.166(3) Uani 1 1 d .
O1W O 0.33828(17) 0.8992(3) 0.2979(2) 0.0612(10) Uani 1 1 d .
O2W O 0.17052(19) 0.6100(3) 0.1798(2) 0.0689(11) Uani 1 1 d .
O3W O 0.4416(2) 0.0207(4) 0.2899(2) 0.0838(13) Uani 1 1 d .
O4W O 0.0851(3) 0.4845(6) 0.2183(5) 0.158(3) Uani 1 1 d .
O16A O 0.38114(16) 0.4676(3) 0.6170(2) 0.0574(10) Uani 1 1 d .
N11A N 0.29828(18) 0.6521(3) 0.3381(2) 0.0428(10) Uani 1 1 d .
C11A C 0.3018(2) 0.5416(5) 0.3309(3) 0.0562(14) Uani 1 1 d .
H11A H 0.2821 0.5086 0.2788 0.067 Uiso 1 1 calc R
C12A C 0.3333(2) 0.4731(4) 0.3975(3) 0.0526(13) Uani 1 1 d .
H12A H 0.3365 0.3961 0.3894 0.063 Uiso 1 1 calc R
C13A C 0.3600(2) 0.5199(4) 0.4758(3) 0.0388(11) Uani 1 1 d .
C14A C 0.3551(2) 0.6348(4) 0.4839(3) 0.0444(12) Uani 1 1 d .
H14A H 0.3722 0.6692 0.5362 0.053 Uiso 1 1 calc R
C15A C 0.3250(2) 0.6973(4) 0.4149(3) 0.0462(12) Uani 1 1 d .
H15A H 0.3227 0.7748 0.4211 0.055 Uiso 1 1 calc R
C16A C 0.3920(2) 0.4510(4) 0.5515(3) 0.0394(11) Uani 1 1 d .
O21A O 0.36596(19) 0.0082(4) 0.4520(2) 0.0723(12) Uani 1 1 d .
N21A N 0.30074(17) -0.1785(3) 0.6702(2) 0.0433(10) Uani 1 1 d .
C21A C 0.3612(2) -0.1687(4) 0.6984(3) 0.0496(13) Uani 1 1 d .
H21A H 0.3829 -0.2020 0.7496 0.059 Uiso 1 1 calc R
C22A C 0.3928(2) -0.1123(4) 0.6560(3) 0.0438(12) Uani 1 1 d .
H22A H 0.4349 -0.1097 0.6772 0.053 Uiso 1 1 calc R
C23A C 0.3604(2) -0.0587(4) 0.5801(3) 0.0406(11) Uani 1 1 d .
C24A C 0.2989(2) -0.0737(4) 0.5505(3) 0.0482(13) Uani 1 1 d .
H24A H 0.2760 -0.0445 0.4982 0.058 Uiso 1 1 calc R
C25A C 0.2711(2) -0.1304(5) 0.5962(3) 0.0546(14) Uani 1 1 d .
H25A H 0.2292 -0.1363 0.5750 0.066 Uiso 1 1 calc R
C26A C 0.3894(2) 0.0070(4) 0.5285(3) 0.0443(12) Uani 1 1 d .
N32A N 0.4400(2) 0.0619(4) 0.5699(3) 0.0527(11) Uani 1 1 d .
H32A H 0.4554 0.0532 0.6236 0.063 Uiso 1 1 calc R
N31A N 0.43153(19) 0.3763(3) 0.5435(2) 0.0473(11) Uani 1 1 d .
H31A H 0.4355 0.3672 0.4952 0.057 Uiso 1 1 calc R
C31A C 0.4685(3) 0.3092(4) 0.6149(3) 0.0546(14) Uani 1 1 d .
H31B H 0.4425 0.2694 0.6393 0.066 Uiso 1 1 calc .
H31C H 0.4947 0.3586 0.6577 0.066 Uiso 1 1 calc .
C32A C 0.5060(2) 0.2263(5) 0.5883(4) 0.0583(15) Uani 1 1 d .
H32B H 0.5335 0.1901 0.6382 0.070 Uiso 1 1 calc .
H32C H 0.5302 0.2669 0.5615 0.070 Uiso 1 1 calc .
C33A C 0.4709(3) 0.1364(5) 0.5289(4) 0.0631(16) Uani 1 1 d .
H33A H 0.4413 0.1715 0.4803 0.076 Uiso 1 1 calc .
H33B H 0.4982 0.0925 0.5094 0.076 Uiso 1 1 calc .
O11B O 0.1481(2) 1.4132(6) 0.3820(3) 0.119(2) Uani 1 1 d .
N11B N 0.21458(17) 1.6450(3) 0.6409(2) 0.0432(10) Uani 1 1 d .
C11B C 0.1541(2) 1.6358(4) 0.6107(3) 0.0460(12) Uani 1 1 d .
H11B H 0.1317 1.6795 0.6349 0.055 Uiso 1 1 calc R
C12B C 0.1244(2) 1.5663(4) 0.5469(3) 0.0493(13) Uani 1 1 d .
H12B H 0.0824 1.5638 0.5276 0.059 Uiso 1 1 calc R
C13B C 0.1561(2) 1.4992(4) 0.5104(3) 0.0480(13) Uani 1 1 d .
C14B C 0.2185(2) 1.5086(5) 0.5402(3) 0.0568(15) Uani 1 1 d .
H14B H 0.2414 1.4666 0.5157 0.068 Uiso 1 1 calc R
C15B C 0.2466(2) 1.5796(5) 0.6058(3) 0.0499(13) Uani 1 1 d .
H15B H 0.2886 1.5830 0.6267 0.060 Uiso 1 1 calc R
C16B C 0.1262(3) 1.4217(6) 0.4384(4) 0.0642(17) Uani 1 1 d .
O26B O 0.11029(18) 0.9456(4) 0.5105(2) 0.0708(12) Uani 1 1 d .
N21B N 0.20729(18) 0.8238(4) 0.3047(2) 0.0445(10) Uani 1 1 d .
C21B C 0.1778(3) 0.7622(5) 0.3447(3) 0.0554(14) Uani 1 1 d .
H21B H 0.1809 0.6841 0.3436 0.066 Uiso 1 1 calc R
C22B C 0.1431(2) 0.8091(5) 0.3877(3) 0.0535(14) Uani 1 1 d .
H22B H 0.1236 0.7633 0.4151 0.064 Uiso 1 1 calc R
C23B C 0.1378(2) 0.9245(4) 0.3893(3) 0.0453(12) Uani 1 1 d .
C24B C 0.1678(2) 0.9884(4) 0.3475(3) 0.0469(12) Uani 1 1 d .
H24B H 0.1645 1.0665 0.3464 0.056 Uiso 1 1 calc R
C25B C 0.2026(2) 0.9359(4) 0.3074(3) 0.0429(12) Uani 1 1 d .
H25B H 0.2236 0.9801 0.2812 0.051 Uiso 1 1 calc R
C26B C 0.1031(2) 0.9771(5) 0.4389(3) 0.0509(13) Uani 1 1 d .
N31B N 0.0759(2) 1.3720(4) 0.4368(3) 0.0628(13) Uani 1 1 d .
H31D H 0.0647 1.3778 0.4799 0.075 Uiso 1 1 calc R
N32B N 0.0653(2) 1.0607(4) 0.4005(3) 0.0574(12) Uani 1 1 d .
H32D H 0.0606 1.0756 0.3488 0.069 Uiso 1 1 calc R
C31B C 0.0384(3) 1.3070(5) 0.3639(4) 0.0709(18) Uani 1 1 d .
H31E H 0.0644 1.2681 0.3390 0.085 Uiso 1 1 calc .
H31F H 0.0129 1.3583 0.3220 0.085 Uiso 1 1 calc .
C32B C -0.0007(3) 1.2223(5) 0.3870(4) 0.0670(17) Uani 1 1 d .
H32E H -0.0286 1.1905 0.3354 0.080 Uiso 1 1 calc .
H32F H -0.0246 1.2617 0.4149 0.080 Uiso 1 1 calc .
C33B C 0.0318(3) 1.1276(5) 0.4425(4) 0.0666(16) Uani 1 1 d .
H33C H 0.0596 1.1578 0.4948 0.080 Uiso 1 1 calc .
H33D H 0.0028 1.0800 0.4558 0.080 Uiso 1 1 calc .
N1G N 0.2518(4) 0.2905(5) 0.0543(4) 0.0919(19) Uani 1 1 d .
O2G O 0.2076(3) 0.3338(6) 0.0029(4) 0.149(3) Uani 1 1 d .
O1G O 0.2959(4) 0.2662(6) 0.0377(4) 0.133(3) Uani 1 1 d .
C1G C 0.2502(3) 0.2699(5) 0.1382(4) 0.0608(15) Uani 1 1 d .
C2G C 0.2968(3) 0.2134(6) 0.1944(4) 0.0740(18) Uani 1 1 d .
H2G H 0.3288 0.1882 0.1787 0.089 Uiso 1 1 calc R
C3G C 0.2969(4) 0.1936(6) 0.2734(4) 0.0779(19) Uani 1 1 d .
H3G H 0.3294 0.1566 0.3125 0.093 Uiso 1 1 calc R
C4G C 0.2495(5) 0.2281(7) 0.2951(5) 0.098(3) Uani 1 1 d .
H4G H 0.2495 0.2150 0.3493 0.118 Uiso 1 1 calc R
C5G C 0.2019(5) 0.2817(8) 0.2382(7) 0.107(3) Uani 1 1 d .
H5G H 0.1693 0.3035 0.2539 0.128 Uiso 1 1 calc R
C6G C 0.2009(3) 0.3036(6) 0.1601(6) 0.093(2) Uani 1 1 d .
H6G H 0.1682 0.3404 0.1215 0.111 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 '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'
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
N11B Cu1 N11A 178.54(17) 4_585 .
N11B Cu1 N21A 89.37(15) 4_585 4_565
N11A Cu1 N21A 90.72(15) . 4_565
N11B Cu1 N21B 89.80(16) 4_585 .
N11A Cu1 N21B 90.16(15) . .
N21A Cu1 N21B 177.89(16) 4_565 .
O102 Cl1 O104 117.7(5) . .
O102 Cl1 O103 103.9(6) . .
O104 Cl1 O103 106.2(4) . .
O102 Cl1 O101 111.7(6) . .
O104 Cl1 O101 110.2(5) . .
O103 Cl1 O101 106.1(6) . .
O202 Cl2 O203 115.0(6) . .
O202 Cl2 O201 108.5(5) . .
O203 Cl2 O201 108.6(4) . .
O202 Cl2 O204 103.6(5) . .
O203 Cl2 O204 109.0(5) . .
O201 Cl2 O204 112.3(5) . .
C15A N11A C11A 117.4(4) . .
C15A N11A Cu1 120.2(3) . .
C11A N11A Cu1 122.4(3) . .
N11A C11A C12A 122.8(5) . .
C13A C12A C11A 119.2(5) . .
C12A C13A C14A 118.1(4) . .
C12A C13A C16A 122.4(4) . .
C14A C13A C16A 119.5(4) . .
C15A C14A C13A 119.4(5) . .
N11A C15A C14A 123.0(5) . .
O16A C16A N31A 124.5(4) . .
O16A C16A C13A 119.0(4) . .
N31A C16A C13A 116.5(4) . .
C25A N21A C21A 116.5(4) . .
C25A N21A Cu1 120.9(3) . 4_566
C21A N21A Cu1 122.4(3) . 4_566
N21A C21A C22A 123.8(4) . .
C21A C22A C23A 118.5(4) . .
C24A C23A C22A 116.8(4) . .
C24A C23A C26A 119.3(4) . .
C22A C23A C26A 123.8(4) . .
C25A C24A C23A 120.9(5) . .
N21A C25A C24A 123.3(5) . .
O21A C26A N32A 123.5(5) . .
O21A C26A C23A 119.5(5) . .
N32A C26A C23A 117.0(4) . .
C26A N32A C33A 123.3(5) . .
C16A N31A C31A 121.4(4) . .
N31A C31A C32A 110.9(5) . .
C31A C32A C33A 115.0(4) . .
N32A C33A C32A 111.2(5) . .
C11B N11B C15B 117.6(4) . .
C11B N11B Cu1 120.6(3) . 4_586
C15B N11B Cu1 121.7(3) . 4_586
N11B C11B C12B 123.2(5) . .
C11B C12B C13B 120.1(5) . .
C12B C13B C14B 117.5(5) . .
C12B C13B C16B 123.0(5) . .
C14B C13B C16B 119.4(5) . .
C15B C14B C13B 120.2(5) . .
N11B C15B C14B 121.4(5) . .
O11B C16B N31B 124.0(5) . .
O11B C16B C13B 118.3(6) . .
N31B C16B C13B 117.6(5) . .
C25B N21B C21B 117.5(4) . .
C25B N21B Cu1 120.2(3) . .
C21B N21B Cu1 122.2(4) . .
N21B C21B C22B 123.2(5) . .
C21B C22B C23B 119.0(5) . .
C24B C23B C22B 118.0(5) . .
C24B C23B C26B 122.1(5) . .
C22B C23B C26B 119.9(5) . .
C25B C24B C23B 119.8(5) . .
N21B C25B C24B 122.5(4) . .
O26B C26B N32B 123.3(5) . .
O26B C26B C23B 120.8(5) . .
N32B C26B C23B 115.9(4) . .
C16B N31B C31B 122.2(5) . .
C26B N32B C33B 123.0(5) . .
N31B C31B C32B 112.4(5) . .
C31B C32B C33B 116.0(5) . .
N32B C33B C32B 110.4(5) . .
O1G N1G O2G 122.1(8) . .
O1G N1G C1G 120.1(7) . .
O2G N1G C1G 117.8(8) . .
C2G C1G C6G 120.2(7) . .
C2G C1G N1G 118.8(6) . .
C6G C1G N1G 121.0(7) . .
C1G C2G C3G 120.2(7) . .
C4G C3G C2G 119.5(8) . .
C5G C4G C3G 120.5(8) . .
C6G C5G C4G 121.3(8) . .
C5G C6G C1G 118.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N11B 2.015(4) 4_585
Cu1 N11A 2.021(4) .
Cu1 N21A 2.022(4) 4_565
Cu1 N21B 2.031(4) .
Cl1 O102 1.304(6) .
Cl1 O104 1.379(5) .
Cl1 O103 1.412(8) .
Cl1 O101 1.387(8) .
Cl2 O202 1.349(6) .
Cl2 O203 1.362(5) .
Cl2 O201 1.376(5) .
Cl2 O204 1.387(7) .
O16A C16A 1.236(5) .
N11A C15A 1.345(6) .
N11A C11A 1.322(6) .
C11A C12A 1.381(7) .
C12A C13A 1.373(6) .
C13A C14A 1.379(7) .
C13A C16A 1.488(6) .
C14A C15A 1.359(6) .
C16A N31A 1.326(6) .
O21A C26A 1.220(5) .
N21A C25A 1.333(6) .
N21A C21A 1.341(6) .
N21A Cu1 2.022(4) 4_566
C21A C22A 1.372(7) .
C22A C23A 1.401(6) .
C23A C24A 1.372(7) .
C23A C26A 1.498(7) .
C24A C25A 1.352(7) .
C26A N32A 1.327(6) .
N32A C33A 1.461(6) .
N31A C31A 1.459(6) .
C31A C32A 1.490(8) .
C32A C33A 1.503(8) .
O11B C16B 1.234(7) .
N11B C11B 1.341(6) .
N11B C15B 1.352(6) .
N11B Cu1 2.015(4) 4_586
C11B C12B 1.346(7) .
C12B C13B 1.375(7) .
C13B C14B 1.383(7) .
C13B C16B 1.495(7) .
C14B C15B 1.369(7) .
C16B N31B 1.315(7) .
O26B C26B 1.222(6) .
N21B C25B 1.336(6) .
N21B C21B 1.341(6) .
C21B C22B 1.384(7) .
C22B C23B 1.376(7) .
C23B C24B 1.386(7) .
C23B C26B 1.493(7) .
C24B C25B 1.378(7) .
C26B N32B 1.342(7) .
N31B C31B 1.465(7) .
N32B C33B 1.464(7) .
C31B C32B 1.501(9) .
C32B C33B 1.495(9) .
N1G O1G 1.199(8) .
N1G O2G 1.216(8) .
N1G C1G 1.453(9) .
C1G C2G 1.357(8) .
C1G C6G 1.393(9) .
C2G C3G 1.357(9) .
C3G C4G 1.351(11) .
C4G C5G 1.359(13) .
C5G C6G 1.338(11) .
