#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/32/4303275.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_4303275
loop_
_publ_author_name
'Mrigendra Dubey'
'Rik Rani Koner'
'Manabendra Ray'
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology Guwahati
Guwahati 781039
;
_publ_contact_author_email       manabray@iitg.ernet.in
_publ_contact_author_name        'Dr. Manabendra Ray'
_publ_section_title
;
Sodium and Potassium Ion Directed Self-Assembled Multinuclear Assembly of
Divalent Nickel or Copper and l-Leucine Derived Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9294
_journal_page_last               9302
_journal_paper_doi               10.1021/ic9011444
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C28 H39 Cu N3 O6, 2(C2 H3 N), 2(C2 N)'
_chemical_formula_sum            'C36 H45 Cu N7 O6'
_chemical_formula_weight         735.34
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 92.053(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.924(2)
_cell_length_b                   9.7748(9)
_cell_length_c                   8.7819(8)
_cell_measurement_reflns_used    2878
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      2.25
_cell_volume                     2052.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Wingx
_computing_publication_material  Wingx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13770
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.9180
_exptl_absorpt_correction_T_min  0.7802
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             774
_exptl_crystal_recrystallization_method 'DMF CH3CN'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.606
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0386P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2926
_reflns_number_total             3578
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic9011444_si_002_7.cif
_cod_data_source_block           Monomer7
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C36 H45 Cu N7 O6 '
_cod_database_code               4303275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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
N2 N 0.0000 0.7609(5) 0.0000 0.0951(16) Uani 1 2 d SDU . .
C15 C 0.0000 0.4987(11) 0.0000 0.222(5) Uani 1 2 d SDU . .
H03A H 0.0161 0.4660 -0.0917 0.334 Uiso 0.50 1 calc PR . .
H03B H -0.0377 0.4660 0.0050 0.334 Uiso 0.50 1 calc PR . .
H03C H 0.0216 0.4660 0.0867 0.334 Uiso 0.50 1 calc PR . .
C14 C 0.0000 0.6506(8) 0.0000 0.098(2) Uani 1 2 d SDU . .
C18 C 0.0000 0.8356(8) 0.5000 0.115(2) Uani 1 2 d S . .
C21 C 0.0000 0.2958(10) 0.5000 0.159(4) Uani 1 2 d S . .
C16 C -0.1232(3) 0.4662(11) 0.2772(8) 0.164(4) Uani 1 1 d D . .
N5 N 0.0390(5) 0.4998(19) 0.3547(12) 0.173(4) Uani 0.50 1 d P . .
N3 N -0.1082(3) 0.3856(10) 0.1948(8) 0.228(4) Uani 1 1 d . . .
C17 C -0.1425(3) 0.5655(9) 0.3783(11) 0.212(4) Uani 1 1 d D . .
H00A H -0.1825 0.5587 0.3835 0.319 Uiso 1 1 calc R . .
H00B H -0.1327 0.6550 0.3428 0.319 Uiso 1 1 calc R . .
H00C H -0.1257 0.5508 0.4778 0.319 Uiso 1 1 calc R . .
C19 C 0.0233(4) 0.7526(14) 0.4189(11) 0.104(3) Uani 0.50 1 d P . .
C20 C 0.0179(5) 0.4030(15) 0.4252(13) 0.124(4) Uani 0.50 1 d P . .
N4 N 0.0466(6) 0.6796(14) 0.3404(13) 0.173(5) Uani 0.50 1 d P . .
Cu1 Cu 0.0000 0.99949(4) 0.0000 0.04958(16) Uani 1 2 d S . .
O1 O 0.04040(7) 1.0168(3) -0.18587(18) 0.0592(6) Uani 1 1 d . . .
O2 O 0.12489(7) 0.9940(4) -0.27873(17) 0.0720(6) Uani 1 1 d . . .
N1 N -0.07581(8) 1.0274(2) -0.1009(2) 0.0440(6) Uani 1 1 d . . .
H1 H -0.0795 0.9713 -0.1832 0.053 Uiso 1 1 calc . . .
C8 C -0.11871(9) 0.9904(4) 0.0106(2) 0.0440(6) Uani 1 1 d . . .
H8 H -0.1498 1.0553 -0.0001 0.053 Uiso 1 1 calc . . .
C13 C 0.09293(10) 1.0027(4) -0.1715(2) 0.0507(6) Uani 1 1 d . . .
C5 C -0.17266(15) 1.2957(4) -0.1898(4) 0.0582(9) Uani 1 1 d . . .
H6 H -0.1672 1.3355 -0.0942 0.070 Uiso 1 1 calc R . .
C7 C -0.07986(12) 1.1727(3) -0.1528(3) 0.0493(7) Uani 1 1 d . . .
H7A H -0.0480 1.1929 -0.2141 0.059 Uiso 1 1 calc R . .
H7B H -0.0776 1.2318 -0.0640 0.059 Uiso 1 1 calc R . .
C6 C -0.13233(12) 1.2062(3) -0.2437(3) 0.0495(7) Uani 1 1 d . . .
C4 C -0.22027(15) 1.3260(4) -0.2758(4) 0.0673(9) Uani 1 1 d . . .
H9 H -0.2469 1.3852 -0.2382 0.081 Uiso 1 1 calc R . .
C9 C -0.14136(12) 0.8464(3) -0.0158(3) 0.0519(7) Uani 1 1 d . . .
H10A H -0.1098 0.7841 -0.0177 0.062 Uiso 1 1 calc R . .
H10B H -0.1632 0.8216 0.0709 0.062 Uiso 1 1 calc R . .
O3 O -0.10179(9) 1.0603(2) -0.4351(2) 0.0653(6) Uani 1 1 d . . .
H11 H -0.1092 1.0367 -0.5232 0.098 Uiso 1 1 calc R . .
C2 C -0.18916(13) 1.1794(4) -0.4738(4) 0.0644(9) Uani 1 1 d . . .
H13 H -0.1948(3) 1.1417(17) -0.568(4) 0.077 Uiso 1 1 calc R . .
C12 C -0.23040(14) 0.9070(4) -0.1614(4) 0.0841(11) Uani 1 1 d . . .
H15A H -0.2498 0.8968 -0.2584 0.126 Uiso 1 1 calc R . .
H15B H -0.2213 1.0016 -0.1449 0.126 Uiso 1 1 calc R . .
H15C H -0.2539 0.8757 -0.0822 0.126 Uiso 1 1 calc R . .
C3 C -0.22826(14) 1.2684(4) -0.4173(4) 0.0717(10) Uani 1 1 d . . .
H16 H -0.2603 1.2895 -0.4758 0.086 Uiso 1 1 calc R . .
C1 C -0.14174(12) 1.1475(3) -0.3881(3) 0.0526(7) Uani 1 1 d . . .
C10 C -0.17727(13) 0.8234(4) -0.1593(3) 0.0600(8) Uani 1 1 d . . .
H19 H -0.1550(7) 0.8525(10) -0.249(3) 0.072 Uiso 1 1 calc R . .
C11 C -0.1903(2) 0.6736(5) -0.1774(6) 0.1077(18) Uani 1 1 d . . .
H22A H -0.2133 0.6444 -0.0961 0.161 Uiso 1 1 calc R . .
H22B H -0.1561 0.6222 -0.1742 0.161 Uiso 1 1 calc R . .
H22C H -0.2098 0.6587 -0.2734 0.161 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 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 '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
C14 N2 Cu1 180.000(1) . . ?
C14 C15 H03A 109.0 . . ?
C14 C15 H03B 109.0 . . ?
H03A C15 H03B 109.0 . . ?
C14 C15 H03C 109.0 . . ?
H03A C15 H03C 110.0 . . ?
H03B C15 H03C 109.0 . . ?
N2 C14 C15 180.000(2) . . ?
C19 C18 C19 97.2(11) . 2_556 ?
C20 C21 C20 74.5(11) . 2_556 ?
N3 C16 C17 179.1(8) . . ?
C20 N5 N4 146.3(11) . . ?
C16 C17 H00A 109.4 . . ?
C16 C17 H00B 109.5 . . ?
H00A C17 H00B 109.5 . . ?
C16 C17 H00C 109.5 . . ?
H00A C17 H00C 109.5 . . ?
H00B C17 H00C 109.5 . . ?
N4 C19 C18 176.9(13) . . ?
N4 C19 C19 141.6(9) . 2_556 ?
C18 C19 C19 41.4(6) . 2_556 ?
N5 C20 C21 174.9(13) . . ?
N5 C20 C20 130.4(8) . 2_556 ?
C21 C20 C20 52.8(5) . 2_556 ?
C19 N4 N5 121.3(12) . . ?
O1 Cu1 O1 169.95(17) 2 . ?
O1 Cu1 N1 83.66(7) 2 . ?
O1 Cu1 N1 94.97(7) . . ?
O1 Cu1 N1 94.97(7) 2 2 ?
O1 Cu1 N1 83.66(7) . 2 ?
N1 Cu1 N1 164.37(13) . 2 ?
O1 Cu1 N2 95.03(9) 2 . ?
O1 Cu1 N2 95.03(9) . . ?
N1 Cu1 N2 97.82(7) . . ?
N1 Cu1 N2 97.82(7) 2 . ?
C13 O1 Cu1 115.52(15) . . ?
C8 N1 C7 113.2(2) . . ?
C8 N1 Cu1 108.05(14) . . ?
C7 N1 Cu1 108.16(16) . . ?
C8 N1 H1 109.1 . . ?
C7 N1 H1 109.1 . . ?
Cu1 N1 H1 109.1 . . ?
N1 C8 C9 112.0(2) . . ?
N1 C8 C13 108.95(19) . 2 ?
C9 C8 C13 110.1(3) . 2 ?
N1 C8 H8 108.6 . . ?
C9 C8 H8 108.6 . . ?
C13 C8 H8 108.6 2 . ?
O2 C13 O1 124.8(2) . . ?
O2 C13 C8 117.3(2) . 2 ?
O1 C13 C8 117.86(18) . 2 ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H6 119.4 . . ?
C6 C5 H6 119.5 . . ?
N1 C7 C6 114.5(2) . . ?
N1 C7 H7A 108.6 . . ?
C6 C7 H7A 108.6 . . ?
N1 C7 H7B 108.6 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C5 C6 C1 118.1(3) . . ?
C5 C6 C7 122.1(3) . . ?
C1 C6 C7 119.8(3) . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H9 120.2 . . ?
C5 C4 H9 120.2 . . ?
C10 C9 C8 116.9(2) . . ?
C10 C9 H10A 108.1 . . ?
C8 C9 H10A 108.1 . . ?
C10 C9 H10B 108.1 . . ?
C8 C9 H10B 108.1 . . ?
H10A C9 H10B 107.3 . . ?
C1 O3 H11 109.5 . . ?
C1 C2 C3 120.1(3) . . ?
C1 C2 H13 120.0 . . ?
C3 C2 H13 119.9 . . ?
C10 C12 H15A 109.5 . . ?
C10 C12 H15B 109.5 . . ?
H15A C12 H15B 109.5 . . ?
C10 C12 H15C 109.5 . . ?
H15A C12 H15C 109.5 . . ?
H15B C12 H15C 109.5 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H16 119.7 . . ?
C2 C3 H16 119.7 . . ?
O3 C1 C2 123.5(3) . . ?
O3 C1 C6 116.1(3) . . ?
C2 C1 C6 120.4(3) . . ?
C11 C10 C12 110.7(3) . . ?
C11 C10 C9 110.0(3) . . ?
C12 C10 C9 112.4(3) . . ?
C11 C10 H19 107.8 . . ?
C12 C10 H19 107.9 . . ?
C9 C10 H19 107.9 . . ?
C10 C11 H22A 109.5 . . ?
C10 C11 H22B 109.5 . . ?
H22A C11 H22B 109.5 . . ?
C10 C11 H22C 109.5 . . ?
H22A C11 H22C 109.5 . . ?
H22B C11 H22C 109.5 . . ?
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
N2 C14 1.079(6) . ?
N2 Cu1 2.332(5) . ?
C15 C14 1.485(12) . ?
C15 H03A 0.9600 . ?
C15 H03B 0.9600 . ?
C15 H03C 0.9600 . ?
C18 C19 1.227(13) . ?
C18 C19 1.227(13) 2_556 ?
C21 C20 1.317(15) . ?
C21 C20 1.317(15) 2_556 ?
C16 N3 1.136(9) . ?
C16 C17 1.406(9) . ?
N5 C20 1.247(18) . ?
N5 N4 1.77(2) . ?
C17 H00A 0.9600 . ?
C17 H00B 0.9600 . ?
C17 H00C 0.9600 . ?
C19 N4 1.151(14) . ?
C19 C19 1.84(2) 2_556 ?
C20 C20 1.59(2) 2_556 ?
Cu1 O1 1.9340(16) 2 ?
Cu1 O1 1.9340(16) . ?
Cu1 N1 2.008(2) . ?
Cu1 N1 2.008(2) 2 ?
O1 C13 1.266(3) . ?
O2 C13 1.237(2) . ?
N1 C8 1.488(3) . ?
N1 C7 1.493(4) . ?
N1 H1 0.9101 . ?
C8 C9 1.523(5) . ?
C8 C13 1.526(3) 2 ?
C8 H8 0.9800 . ?
C13 C8 1.526(3) 2 ?
C5 C4 1.376(5) . ?
C5 C6 1.398(4) . ?
C5 H6 0.9300 . ?
C7 C6 1.499(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 C1 1.402(4) . ?
C4 C3 1.371(5) . ?
C4 H9 0.9300 . ?
C9 C10 1.516(4) . ?
C9 H10A 0.9700 . ?
C9 H10B 0.9700 . ?
O3 C1 1.356(3) . ?
O3 H11 0.8200 . ?
C2 C1 1.375(4) . ?
C2 C3 1.383(5) . ?
C2 H13 0.9129 . ?
C12 C10 1.511(5) . ?
C12 H15A 0.9600 . ?
C12 H15B 0.9600 . ?
C12 H15C 0.9600 . ?
C3 H16 0.9300 . ?
C10 C11 1.504(5) . ?
C10 H19 1.0058 . ?
C11 H22A 0.9600 . ?
C11 H22B 0.9600 . ?
C11 H22C 0.9600 . ?
