#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:22:48 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179575 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/40/4504030.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_4504030
loop_
_publ_author_name
'Kumar, D. Krishna'
'Das, Amitava'
'Dastidar, Parthasarathi'
_publ_section_title
;
 Remarkably Stable Porous Assembly of Nanorods Derived from a Simple
 Metal−Organic Framework
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              205
_journal_paper_doi               10.1021/cg0606693
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C11 H18 Cu N4 O9 S'
_chemical_formula_weight         445.89
_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                 122.872(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5168(8)
_cell_length_b                   21.771(2)
_cell_length_c                   12.1053(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1663.8(3)
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_collection       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_molecular_graphics    'PLATON, MERCURY 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6502
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0478
_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)+(0.0586P)²+7.4715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                1754
_reflns_number_total             2163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0606693si20061003_010527.cif
_cod_data_source_block           kkb354dm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4504030
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 0.81377(10) 0.20909(3) 1.00988(7) 0.0193(3) Uani 1 1 d .
N1 N 0.8761(7) 0.1230(2) 1.0768(4) 0.0146(10) Uani 1 1 d .
C2 C 1.0373(9) 0.1120(2) 1.1990(5) 0.0185(13) Uani 1 1 d .
H2 H 1.1152 0.1451 1.2520 0.022 Uiso 1 1 calc R
C3 C 1.0933(9) 0.0535(3) 1.2499(5) 0.0210(13) Uani 1 1 d .
H3 H 1.2080 0.0471 1.3353 0.025 Uiso 1 1 calc R
C4 C 0.9760(9) 0.0046(2) 1.1717(5) 0.0170(13) Uani 1 1 d .
H4 H 1.0124 -0.0353 1.2040 0.020 Uiso 1 1 calc R
C5 C 0.8046(8) 0.0148(2) 1.0455(5) 0.0138(12) Uani 1 1 d .
C6 C 0.7589(8) 0.0756(2) 0.9992(5) 0.0156(12) Uani 1 1 d .
H6 H 0.6461 0.0834 0.9138 0.019 Uiso 1 1 calc R
N7 N 0.6882(7) -0.03596(19) 0.9701(4) 0.0161(11) Uani 1 1 d .
H7 H 0.7235 -0.0708 1.0101 0.019 Uiso 1 1 calc R
C8 C 0.5268(8) -0.0373(2) 0.8419(5) 0.0157(12) Uani 1 1 d .
O9 O 0.4482(6) 0.00848(16) 0.7720(3) 0.0181(9) Uani 1 1 d .
N10 N 0.4598(7) -0.0962(2) 0.7972(4) 0.0222(12) Uani 1 1 d .
H10 H 0.5163 -0.1250 0.8549 0.027 Uiso 1 1 calc R
C11 C 0.3107(8) -0.1142(3) 0.6689(5) 0.0200(13) Uani 1 1 d .
C12 C 0.3153(9) -0.1757(3) 0.6390(6) 0.0278(15) Uani 1 1 d .
H12 H 0.4175 -0.2010 0.7050 0.033 Uiso 1 1 calc R
N13 N 0.1825(7) -0.2003(2) 0.5222(5) 0.0272(13) Uani 1 1 d .
C14 C 0.0361(9) -0.1640(3) 0.4256(6) 0.0232(14) Uani 1 1 d .
H14 H -0.0563 -0.1807 0.3427 0.028 Uiso 1 1 calc R
C15 C 0.0201(8) -0.1027(2) 0.4466(5) 0.0186(13) Uani 1 1 d .
H15 H -0.0827 -0.0784 0.3785 0.022 Uiso 1 1 calc R
C16 C 0.1569(8) -0.0774(2) 0.5693(5) 0.0187(13) Uani 1 1 d .
H16 H 0.1459 -0.0361 0.5847 0.022 Uiso 1 1 calc R
O17 O 0.9102(6) 0.18881(18) 0.8903(4) 0.0309(11) Uani 1 1 d .
S18 S 1.1380(3) 0.20378(9) 0.9488(2) 0.0476(6) Uani 1 1 d .
O19 O 1.2430(7) 0.2102(3) 1.0916(5) 0.071(2) Uani 1 1 d .
O20 O 1.2344(9) 0.1539(2) 0.9169(7) 0.085(2) Uani 1 1 d .
O21 O 1.1497(6) 0.26126(19) 0.8884(4) 0.0304(11) Uani 1 1 d .
O22 O 0.4893(6) 0.19319(17) 0.8391(4) 0.0200(9) Uani 1 1 d .
O23 O 0.7644(6) 0.22819(17) 1.1514(4) 0.0247(10) Uani 1 1 d .
O24 O 0.5000(7) 0.1758(2) 0.6011(4) 0.0497(14) Uani 1 1 d .
O25 O 0.5218(8) 0.0498(3) 0.5810(4) 0.0595(16) Uani 1 1 d .
H22A H 0.3982 0.1837 0.8593 0.050 Uiso 1 1 d .
H22B H 0.4389 0.1861 0.7558 0.050 Uiso 1 1 d .
H23A H 0.6757 0.2623 1.1408 0.050 Uiso 1 1 d .
H23B H 0.9062 0.2286 1.2319 0.050 Uiso 1 1 d .
H24A H 0.3709 0.1918 0.5317 0.050 Uiso 1 1 d .
H24B H 0.4693 0.1388 0.5823 0.050 Uiso 1 1 d .
H25A H 0.4730 0.0452 0.6429 0.050 Uiso 1 1 d .
H25B H 0.4730 0.0299 0.5251 0.050 Uiso 1 1 d .
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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 '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'
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
O23 Cu1 O17 171.14(17) . .
O23 Cu1 N1 87.66(17) . .
O17 Cu1 N1 89.37(17) . .
O23 Cu1 N13 89.43(19) . 2_656
O17 Cu1 N13 91.61(19) . 2_656
N1 Cu1 N13 166.99(18) . 2_656
O23 Cu1 O22 102.25(14) . .
O17 Cu1 O22 86.41(16) . .
N1 Cu1 O22 97.45(16) . .
N13 Cu1 O22 95.56(16) 2_656 .
C2 N1 C6 119.6(5) . .
C2 N1 Cu1 119.5(4) . .
C6 N1 Cu1 120.9(3) . .
N1 C2 C3 122.4(5) . .
N1 C2 H2 118.8 . .
C3 C2 H2 118.8 . .
C2 C3 C4 118.7(5) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C3 C4 C5 120.1(5) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C4 C5 N7 118.3(5) . .
C4 C5 C6 118.1(5) . .
N7 C5 C6 123.6(5) . .
N1 C6 C5 121.0(5) . .
N1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C8 N7 C5 128.2(4) . .
C8 N7 H7 115.9 . .
C5 N7 H7 115.9 . .
O9 C8 N7 124.5(5) 1 .
O9 C8 N7 124.5(5) . .
O9 C8 N10 123.2(5) 1 .
O9 C8 N10 123.2(5) . .
N7 C8 N10 112.3(5) . .
O9 O9 C8 0(10) 1 .
C8 N10 C11 127.1(5) . .
C8 N10 H10 116.5 . .
C11 N10 H10 116.5 . .
C16 C11 N10 126.6(5) . .
C16 C11 C12 117.2(5) . .
N10 C11 C12 116.2(5) . .
N13 C12 C11 123.7(5) . .
N13 C12 H12 118.1 . .
C11 C12 H12 118.1 . .
C12 N13 C14 118.7(5) . .
C12 N13 Cu1 121.4(4) . 2_646
C14 N13 Cu1 119.9(4) . 2_646
N13 C14 C15 121.4(5) . .
N13 C14 H14 119.3 . .
C15 C14 H14 119.3 . .
C14 C15 C16 119.8(5) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C15 C16 C11 119.1(5) . .
C15 C16 H16 120.4 . .
C11 C16 H16 120.4 . .
S18 O17 Cu1 112.6(3) . .
O19 S18 O20 110.7(4) . .
O19 S18 O21 111.4(3) . .
O20 S18 O21 109.0(3) . .
O19 S18 O17 109.1(3) . .
O20 S18 O17 108.5(3) . .
O21 S18 O17 108.2(2) . .
Cu1 O22 H22A 114.4(3) . .
Cu1 O22 H22B 132.3(3) . .
H22A O22 H22B 111.6(4) . .
Cu1 O23 H23A 119.3(3) . .
Cu1 O23 H23B 104.4(3) . .
H23A O23 H23B 115.3(4) . .
H24A O24 H24B 96.7(4) . .
H25A O25 H25B 116.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O23 1.984(4) .
Cu1 O17 1.989(4) .
Cu1 N1 1.995(4) .
Cu1 N13 2.015(5) 2_656
Cu1 O22 2.207(4) .
N1 C2 1.329(7) .
N1 C6 1.350(7) .
C2 C3 1.378(8) .
C2 H2 0.9300 .
C3 C4 1.378(8) .
C3 H3 0.9300 .
C4 C5 1.381(8) .
C4 H4 0.9300 .
C5 N7 1.397(7) .
C5 C6 1.406(7) .
C6 H6 0.9300 .
N7 C8 1.355(7) .
N7 H7 0.8600 .
C8 O9 1.231(6) 1
C8 O9 1.231(6) .
C8 N10 1.377(7) .
N10 C11 1.390(7) .
N10 H10 0.8600 .
C11 C16 1.386(8) .
C11 C12 1.394(8) .
C12 N13 1.322(7) .
C12 H12 0.9300 .
N13 C14 1.344(7) .
N13 Cu1 2.015(5) 2_646
C14 C15 1.375(8) .
C14 H14 0.9300 .
C15 C16 1.381(8) .
C15 H15 0.9300 .
C16 H16 0.9300 .
O17 S18 1.491(4) .
S18 O19 1.465(6) .
S18 O20 1.469(6) .
S18 O21 1.476(4) .
O22 H22A 0.868(3) .
O22 H22B 0.877(4) .
O23 H23A 0.959(4) .
O23 H23B 0.979(4) .
O24 H24A 0.940(5) .
O24 H24B 0.834(5) .
O25 H25A 1.003(5) .
O25 H25B 0.715(6) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N7 H7 O20 0.86 1.96 2.818(6) 172.3 3_757
N10 H10 O19 0.86 2.42 3.113(7) 138.1 3_757
N10 H10 O20 0.86 2.43 3.195(8) 147.9 3_757
O22 H22A O20 0.868(3) 1.832(4) 2.692(6) 171.1(3) 1_455
O22 H22B O24 0.877(4) 2.169(5) 2.950(6) 148.1(3) 1
O23 H23A O24 0.959(4) 1.762(4) 2.717(5) 173.2(3) 4_566
O23 H23B O21 0.979(4) 1.795(4) 2.766(5) 170.8(3) 4_566
O24 H24A O21 0.940(5) 1.920(4) 2.843(6) 166.5(3) 4_465
O24 H24B O25 0.834(5) 1.979(6) 2.765(8) 156.9(4) 1
O25 H25A O9 1.003(5) 1.853(4) 2.802(6) 156.8(3) 1
C2 H2 O21 0.93 2.55 3.388(7) 150.7 4_566
O25 H25B O25 0.715(6) 2.172(6) 2.821(12) 151.6(3) 3_656
C3 H3 O25 0.93 2.61 3.526(7) 169.8 1_656
C12 H12 O19 0.93 2.41 3.235(7) 148.3 3_757
