#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/04/7050449.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_7050449
loop_
_publ_author_name
'Sain, Saugata'
'Kumar Maji, Tapas'
'Mostafa, Golam'
'Lu, Tian-Huey'
'Ray Chaudhuri, Nirmalendu'
_publ_section_title
;
 A novel layered and pillared topology in a 3D open framework:
 synthesis, crystal structure and magnetic propertiesElectronic
 supplementary information (ESI) available: Fig. S1: showing the
 brick-walled shaped view of the [{Cu3(malonate)2(H2O)2}]n layer; Fig.
 S2: space-filled diagram showing channels viewed down x-axis. See
 http://www.rsc.org/suppdata/nj/b2/b208650f/
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              185
_journal_paper_doi               10.1039/b208650f
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C42 H44 Cu3 N6 O10, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C42 H48 Cu3 N8 O18'
_chemical_formula_weight         1143.53
_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                 91.352(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3890(14)
_cell_length_b                   16.3111(16)
_cell_length_c                   10.9990(11)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_volume                     2401.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_computing_publication_material  'Platon99 (Spek, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14940
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  0.95908
_exptl_absorpt_correction_T_min  0.82258
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5727
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0482P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                3109
_reflns_number_total             5727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208650f.txt
_cod_data_source_block           CIF_of_Complex_1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7050449
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.49386(3) 0.24003(2) 0.80452(4) 0.02468(13) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 1.0000 0.0570(3) Uani 1 2 d SD . .
N1 N 0.6463(2) 0.24343(17) 0.8059(3) 0.0330(7) Uani 1 1 d . . .
N2 N 0.3418(2) 0.23397(18) 0.7897(3) 0.0351(7) Uani 1 1 d . . .
O1 O 0.49081(17) 0.34345(13) 0.7112(2) 0.0284(6) Uani 1 1 d . A .
O2 O 0.5010(2) 0.41238(15) 0.8781(3) 0.0589(9) Uani 1 1 d . A .
O3 O 0.5046(2) 0.58980(15) 0.8431(2) 0.0534(9) Uani 1 1 d . A .
O4 O 0.50129(16) 0.62442(13) 0.6502(2) 0.0278(6) Uani 1 1 d . . .
O1W O 0.4892(2) 0.26054(14) 1.0067(2) 0.0453(7) Uani 1 1 d . . .
H1W1 H 0.4790 0.2165 1.0583 0.054 Uiso 1 1 d . . .
H2W1 H 0.4868 0.2942 1.0556 0.054 Uiso 1 1 d . . .
C1 C 0.6981(3) 0.1968(3) 0.8855(4) 0.0488(12) Uani 1 1 d . . .
H1 H 0.6611 0.1583 0.9368 0.059 Uiso 1 1 d . . .
C2 C 0.8002(3) 0.2003(3) 0.9011(5) 0.0601(14) Uani 1 1 d . . .
H2 H 0.8373 0.1477 0.9494 0.072 Uiso 1 1 d . . .
C3 C 0.8551(3) 0.2536(3) 0.8335(4) 0.0534(12) Uani 1 1 d . . .
C4 C 0.8022(3) 0.3010(3) 0.7487(5) 0.0623(14) Uani 1 1 d . . .
H4 H 0.8377 0.3361 0.6826 0.075 Uiso 1 1 d . . .
C5 C 0.7007(3) 0.2942(3) 0.7386(4) 0.0491(12) Uani 1 1 d . . .
H5 H 0.6656 0.3239 0.6756 0.059 Uiso 1 1 d . . .
C6 C 0.9680(3) 0.2615(3) 0.8492(5) 0.0664(14) Uani 1 1 d . . .
H6A H 0.9956 0.2333 0.9150 0.080 Uiso 1 1 d . . .
H6B H 0.9873 0.3294 0.8266 0.080 Uiso 1 1 d . . .
C7 C 0.0182(3) 0.2082(3) 0.7583(5) 0.0632(14) Uani 1 1 d . . .
H7A H 0.0025 0.1436 0.7806 0.076 Uiso 1 1 d . . .
H7B H -0.0040 0.2240 0.6629 0.076 Uiso 1 1 d . . .
C8 C 0.1325(3) 0.2177(3) 0.7698(5) 0.0555(12) Uani 1 1 d . . .
C9 C 0.1838(3) 0.2746(3) 0.7038(5) 0.0702(16) Uani 1 1 d . . .
H9 H 0.1451 0.3078 0.6429 0.084 Uiso 1 1 d . . .
C10 C 0.2859(3) 0.2807(3) 0.7138(4) 0.0549(13) Uani 1 1 d . . .
H10 H 0.3231 0.3194 0.6571 0.066 Uiso 1 1 d . . .
C11 C 0.2921(3) 0.1800(3) 0.8582(4) 0.0537(12) Uani 1 1 d . . .
H11 H 0.3331 0.1485 0.9416 0.064 Uiso 1 1 d . . .
C12 C 0.1892(3) 0.1710(3) 0.8507(5) 0.0683(15) Uani 1 1 d . . .
H12 H 0.1601 0.1346 0.9185 0.082 Uiso 1 1 d . . .
C13 C 0.4970(3) 0.4106(2) 0.7674(3) 0.0278(8) Uani 1 1 d . . .
C14 C 0.5002(4) 0.4847(2) 0.6859(4) 0.0492(12) Uani 1 1 d . A .
H14A H 0.4451 0.4947 0.5993 0.059 Uiso 1 1 d . . .
H14B H 0.5863 0.4804 0.6407 0.059 Uiso 1 1 d . . .
C15 C 0.5024(3) 0.5716(2) 0.7342(3) 0.0271(8) Uani 1 1 d . . .
N3 N 0.3606(3) 0.5019(3) 0.9873(4) 0.0487(14) Uani 0.65 1 d PG A 1
C16 C 0.3121(4) 0.5763(2) 0.9679(5) 0.072(2) Uani 0.65 1 d PG A 1
H16 H 0.3488 0.6246 0.9649 0.086 Uiso 0.65 1 calc PR A 1
C17 C 0.2088(4) 0.5784(3) 0.9529(6) 0.088(3) Uani 0.65 1 d PG A 1
H17 H 0.1763 0.6282 0.9400 0.106 Uiso 0.65 1 calc PR A 1
C18 C 0.1539(3) 0.5062(4) 0.9574(6) 0.087(3) Uani 0.65 1 d PG A 1
C19 C 0.2024(4) 0.4318(3) 0.9768(6) 0.098(3) Uani 0.65 1 d PG A 1
H19 H 0.1657 0.3835 0.9798 0.118 Uiso 0.65 1 calc PR A 1
C20 C 0.3057(4) 0.4297(2) 0.9918(5) 0.075(2) Uani 0.65 1 d PG A 1
H20 H 0.3381 0.3799 1.0048 0.090 Uiso 0.65 1 calc PR A 1
C21 C 0.0344(8) 0.5074(6) 0.9364(9) 0.121(4) Uani 0.65 1 d P . 1
H21A H 0.0166 0.4652 0.8777 0.145 Uiso 0.65 1 calc PR . 1
H21B H 0.0157 0.5598 0.9008 0.145 Uiso 0.65 1 calc PR . 1
N3A N 0.3264(4) 0.5034(4) 0.9925(7) 0.043(2) Uani 0.35 1 d PGD A 2
C16A C 0.2743(6) 0.5024(5) 1.1003(5) 0.065(4) Uani 0.35 1 d PG A 2
H16A H 0.3089 0.5001 1.1746 0.078 Uiso 0.35 1 calc PR A 2
C17A C 0.1705(6) 0.5050(6) 1.0971(8) 0.077(5) Uani 0.35 1 d PG A 2
H17A H 0.1356 0.5043 1.1693 0.092 Uiso 0.35 1 calc PR A 2
C18A C 0.1188(4) 0.5085(6) 0.9862(10) 0.076(5) Uani 0.35 1 d PGD A 2
C19A C 0.1709(6) 0.5095(6) 0.8784(8) 0.080(5) Uani 0.35 1 d PG A 2
H19A H 0.1363 0.5119 0.8041 0.096 Uiso 0.35 1 calc PR A 2
C20A C 0.2747(6) 0.5069(5) 0.8815(6) 0.061(4) Uani 0.35 1 d PG A 2
H20A H 0.3096 0.5076 0.8094 0.073 Uiso 0.35 1 calc PR A 2
C21A C 0.0089(12) 0.5313(11) 0.979(2) 0.108(7) Uani 0.35 1 d PD . 2
H21C H -0.0084 0.5776 1.0297 0.130 Uiso 0.35 1 calc PR . 2
H21D H -0.0172 0.5383 0.8966 0.130 Uiso 0.35 1 calc PR . 2
N5 N 0.2297(5) 0.5013(3) 0.5134(6) 0.0834(16) Uani 1 1 d . B 3
O5 O 0.2701(5) 0.5362(3) 0.4354(5) 0.143(2) Uani 1 1 d . B 3
O6 O 0.1393(5) 0.5079(3) 0.5209(7) 0.187(3) Uani 1 1 d . B 3
O7 O 0.2701(5) 0.4622(3) 0.5842(6) 0.170(3) Uani 1 1 d . B 3
O2W O 0.0035(4) 0.5814(4) 0.3630(6) 0.202(3) Uani 1 1 d . C 3
H1W2 H 0.0541 0.5577 0.3981 0.242 Uiso 1 1 d . D 3
H2W2 H -0.0485 0.5590 0.3938 0.242 Uiso 1 1 d . E 3
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'
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
_geom_angle_publ_flag
O4 Cu1 O1 163.46(10) 2_646 . ?
O4 Cu1 N1 89.84(10) 2_646 . ?
O1 Cu1 N1 89.37(11) . . ?
O4 Cu1 N2 90.04(11) 2_646 . ?
O1 Cu1 N2 89.51(11) . . ?
N1 Cu1 N2 175.67(13) . . ?
O4 Cu1 O1W 83.85(9) 2_646 . ?
O1 Cu1 O1W 112.69(9) . . ?
N1 Cu1 O1W 92.28(11) . . ?
N2 Cu1 O1W 92.01(12) . . ?
N3 Cu2 N3 180.0 . 3_667 ?
N3 Cu2 O2 90.93(16) . 3_667 ?
N3 Cu2 O2 89.07(16) 3_667 3_667 ?
N3 Cu2 O2 89.07(17) . . ?
N3 Cu2 O2 90.93(16) 3_667 . ?
O2 Cu2 O2 180.000(1) 3_667 . ?
N3 Cu2 O3 88.68(16) . . ?
N3 Cu2 O3 91.32(16) 3_667 . ?
O2 Cu2 O3 92.89(10) 3_667 . ?
O2 Cu2 O3 87.11(10) . . ?
N3 Cu2 O3 91.32(16) . 3_667 ?
N3 Cu2 O3 88.68(16) 3_667 3_667 ?
O2 Cu2 O3 87.11(10) 3_667 3_667 ?
O2 Cu2 O3 92.89(10) . 3_667 ?
O3 Cu2 O3 180.000(1) . 3_667 ?
N3 Cu2 N3A 2.30(18) . . ?
N3 Cu2 N3A 177.70(18) 3_667 . ?
O2 Cu2 N3A 89.1(2) 3_667 . ?
O2 Cu2 N3A 90.9(2) . . ?
O3 Cu2 N3A 90.1(2) . . ?
O3 Cu2 N3A 89.9(2) 3_667 . ?
N3 Cu2 N3A 177.70(18) . 3_667 ?
N3 Cu2 N3A 2.30(18) 3_667 3_667 ?
O2 Cu2 N3A 90.9(2) 3_667 3_667 ?
O2 Cu2 N3A 89.1(2) . 3_667 ?
O3 Cu2 N3A 89.9(2) . 3_667 ?
O3 Cu2 N3A 90.1(2) 3_667 3_667 ?
N3A Cu2 N3A 180.0 . 3_667 ?
C5 N1 C1 115.6(3) . . ?
C5 N1 Cu1 124.8(3) . . ?
C1 N1 Cu1 119.5(3) . . ?
C10 N2 C11 116.3(3) . . ?
C10 N2 Cu1 124.2(3) . . ?
C11 N2 Cu1 119.5(3) . . ?
C13 O1 Cu1 119.2(2) . . ?
C13 O2 Cu2 134.5(2) . . ?
C15 O3 Cu2 125.7(2) . . ?
C15 O4 Cu1 118.2(2) . 2_656 ?
N1 C1 C2 123.8(4) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C3 C4 116.4(4) . . ?
C2 C3 C6 122.4(4) . . ?
C4 C3 C6 121.1(4) . . ?
C5 C4 C3 120.0(4) . . ?
N1 C5 C4 124.0(4) . . ?
C7 C6 C3 109.6(4) 1_655 . ?
C6 C7 C8 110.3(4) 1_455 . ?
C9 C8 C12 116.0(4) . . ?
C9 C8 C7 122.2(4) . . ?
C12 C8 C7 121.8(4) . . ?
C8 C9 C10 121.1(4) . . ?
N2 C10 C9 123.2(4) . . ?
N2 C11 C12 122.7(4) . . ?
C11 C12 C8 120.6(4) . . ?
O2 C13 O1 120.8(3) . . ?
O2 C13 C14 125.0(3) . . ?
O1 C13 C14 114.1(3) . . ?
C13 C14 C15 122.9(3) . . ?
O3 C15 O4 123.0(3) . . ?
O3 C15 C14 124.5(3) . . ?
O4 C15 C14 112.5(3) . . ?
C16 N3 C20 120.0 . . ?
C16 N3 Cu2 119.2(3) . . ?
C20 N3 Cu2 120.7(3) . . ?
N3 C16 C17 120.0 . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 C21 119.4(5) . . ?
C17 C18 C21 120.5(5) . . ?
C18 C19 C20 120.0 . . ?
C19 C20 N3 120.0 . . ?
C18 C21 C21 115.6(9) . 3_567 ?
C16A N3A C20A 120.0 . . ?
C16A N3A Cu2 119.4(4) . . ?
C20A N3A Cu2 120.6(4) . . ?
C17A C16A N3A 120.0 . . ?
C16A C17A C18A 120.0 . . ?
C19A C18A C17A 120.0 . . ?
C19A C18A C21A 117.3(11) . . ?
C17A C18A C21A 121.2(11) . . ?
C20A C19A C18A 120.0 . . ?
C19A C20A N3A 120.0 . . ?
C21A C21A C18A 88.4(18) 3_567 . ?
O7 N5 O5 123.7(8) . . ?
O7 N5 O6 117.4(8) . . ?
O5 N5 O6 118.9(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.951(2) 2_646 ?
Cu1 O1 1.974(2) . ?
Cu1 N1 2.041(3) . ?
Cu1 N2 2.041(3) . ?
Cu1 O1W 2.251(3) . ?
Cu2 N3 1.869(4) . ?
Cu2 N3 1.869(4) 3_667 ?
Cu2 O2 1.960(3) 3_667 ?
Cu2 O2 1.960(3) . ?
Cu2 O3 2.265(3) . ?
Cu2 O3 2.265(3) 3_667 ?
Cu2 N3A 2.325(6) . ?
Cu2 N3A 2.325(6) 3_667 ?
N1 C5 1.338(5) . ?
N1 C1 1.341(5) . ?
N2 C10 1.344(5) . ?
N2 C11 1.346(5) . ?
O1 C13 1.259(4) . ?
O2 C13 1.218(4) . ?
O3 C15 1.234(4) . ?
O4 C15 1.264(4) . ?
O4 Cu1 1.951(2) 2_656 ?
C1 C2 1.374(5) . ?
C2 C3 1.370(6) . ?
C3 C4 1.391(6) . ?
C3 C6 1.523(5) . ?
C4 C5 1.366(5) . ?
C6 C7 1.496(7) 1_655 ?
C7 C6 1.496(7) 1_455 ?
C7 C8 1.541(6) . ?
C8 C9 1.372(6) . ?
C8 C12 1.384(6) . ?
C9 C10 1.373(6) . ?
C11 C12 1.385(6) . ?
C13 C14 1.505(5) . ?
C14 C15 1.514(5) . ?
N3 C16 1.3900 . ?
N3 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C21 1.611(11) . ?
C19 C20 1.3900 . ?
C21 C21 1.71(2) 3_567 ?
N3A C16A 1.3900 . ?
N3A C20A 1.3900 . ?
C16A C17A 1.3900 . ?
C17A C18A 1.3900 . ?
C18A C19A 1.3900 . ?
C18A C21A 1.517(16) . ?
C19A C20A 1.3900 . ?
C21A C21A 1.15(3) 3_567 ?
N5 O7 1.134(6) . ?
N5 O5 1.172(7) . ?
N5 O6 1.220(7) . ?
