#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:35:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180188 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/84/7108441.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_7108441
loop_
_publ_author_name
'Gao-Chao Lv'
'Peng Wang'
'Qing Liu'
Jian
Fan
'Kai Chen'
'Wei-Yin Sun'
_publ_section_title
;
 Unprecedented crystal dynamics: reversible cascades of
 single-crystal-to-single-crystal transformations
;
_journal_name_full               Chem.Commun.
_journal_page_first              10249
_journal_paper_doi               10.1039/c2cc35456j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C29 H45 Cu N13 O8'
_chemical_formula_weight         767.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.067(2)
_cell_length_b                   15.675(5)
_cell_length_c                   18.811(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2083.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11588
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.9442
_exptl_absorpt_correction_T_min  0.8449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
This unit cell contains 14 methanol molecules which have been treated
as a diffuse contribution to the overall scattering without specific
atom positions by squeeze/platon.
;
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2094
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0842P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                1307
_reflns_number_total             2094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35456j.txt
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      Pmma
_cod_database_code               7108441
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z'
'-x, y, -z'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, y, z'
'x, -y, 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
Cu1 Cu 0.5000 0.0000 0.0000 0.0556(3) Uani 1 4 d S
N1 N 0.4074(3) 0.15559(13) 0.08242(13) 0.0640(6) Uani 1 1 d .
N2 N 0.3433(3) 0.08890(12) 0.04673(11) 0.0568(6) Uani 1 1 d .
N3 N 0.2500 0.5360(16) 0.6701(3) 0.305(18) Uani 1 2 d SD
N4 N 0.2500 0.5687(7) 0.6036(3) 0.229(6) Uani 1 2 d SD
N5 N 0.2500 0.5000 0.2663(3) 0.0774(16) Uani 1 4 d S
C1 C 0.2500 0.1957(2) 0.1040(2) 0.0626(11) Uani 1 2 d S
C2 C 0.2500 0.2745(2) 0.1470(2) 0.0646(11) Uani 1 2 d S
C3 C 0.0900(6) 0.3106(3) 0.1686(3) 0.1391(19) Uani 1 1 d .
H3 H -0.0249 0.2855 0.1566 0.167 Uiso 1 1 calc R
C4 C 0.0909(7) 0.3848(3) 0.2085(3) 0.1390(19) Uani 1 1 d .
H4 H -0.0236 0.4085 0.2228 0.167 Uiso 1 1 calc R
C5 C 0.2500 0.4226(2) 0.2267(2) 0.0710(12) Uani 1 2 d S
C6 C 0.2500 0.5000 0.3386(3) 0.0638(16) Uani 1 4 d S
C7 C 0.2500 0.5763(3) 0.3783(3) 0.0890(15) Uani 1 2 d S
H7 H 0.2500 0.6284 0.3547 0.107 Uiso 1 2 calc SR
C8 C 0.2500 0.5748(4) 0.4520(3) 0.1001(17) Uani 1 2 d S
H8 H 0.2500 0.6263 0.4766 0.120 Uiso 1 2 calc SR
C9 C 0.2500 0.5000 0.4896(4) 0.099(3) Uani 1 4 d S
C10 C 0.2500 0.5000 0.5620(6) 0.128(4) Uani 1 4 d S
O1 O 0.2500 0.0000 -0.0922(3) 0.0937(15) Uani 1 4 d S
C11 C 0.2500 0.0000 -0.1568(6) 0.260(11) Uani 1 4 d S
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'
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'
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
N2 Cu1 N2 89.16(11) 8 .
N2 Cu1 N2 180.00(16) 8 4_655
N2 Cu1 N2 90.84(11) . 4_655
N2 Cu1 N2 90.84(11) 8 5_655
N2 Cu1 N2 180.00(16) . 5_655
N2 Cu1 N2 89.16(11) 4_655 5_655
N2 N1 C1 103.9(2) . .
N2 N2 N1 110.03(13) 7_655 .
N2 N2 Cu1 123.91(6) 7_655 .
N1 N2 Cu1 126.06(16) . .
N3 N3 N4 112.3(10) 2_565 .
C10 N4 N3 103.7(11) . .
C6 N5 C5 121.5(2) . .
C6 N5 C5 121.5(2) . 2_565
C5 N5 C5 116.9(5) . 2_565
N1 C1 N1 112.1(3) 7_655 .
N1 C1 C2 123.96(16) 7_655 .
N1 C1 C2 123.96(16) . .
C3 C2 C3 116.7(4) 7_655 .
C3 C2 C1 121.6(2) 7_655 .
C3 C2 C1 121.6(2) . .
C2 C3 C4 121.4(4) . .
C2 C3 H3 119.3 . .
C4 C3 H3 119.3 . .
C5 C4 C3 121.5(4) . .
C5 C4 H4 119.2 . .
C3 C4 H4 119.2 . .
C4 C5 C4 117.4(5) . 7_655
C4 C5 N5 121.3(2) . .
C4 C5 N5 121.3(2) 7_655 .
N5 C6 C7 122.0(3) . 2_565
N5 C6 C7 122.0(3) . .
C7 C6 C7 116.1(6) 2_565 .
C8 C7 C6 121.0(5) . .
C8 C7 H7 119.5 . .
C6 C7 H7 119.5 . .
C9 C8 C7 122.1(6) . .
C9 C8 H8 119.0 . .
C7 C8 H8 119.0 . .
C10 C9 C8 121.1(4) . .
C10 C9 C8 121.1(4) . 2_565
C8 C9 C8 117.8(7) . 2_565
N4 C10 N4 108.0(10) . 2_565
N4 C10 C9 126.0(5) . .
N4 C10 C9 126.0(5) 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.985(2) 8
Cu1 N2 1.985(2) .
Cu1 N2 1.985(2) 4_655
Cu1 N2 1.985(2) 5_655
N1 N2 1.322(3) .
N1 C1 1.341(3) .
N2 N2 1.318(4) 7_655
N3 N3 1.13(5) 2_565
N3 N4 1.352(9) .
N4 C10 1.331(9) .
N5 C6 1.360(7) .
N5 C5 1.424(5) .
N5 C5 1.424(5) 2_565
C1 N1 1.341(3) 7_655
C1 C2 1.475(5) .
C2 C3 1.328(4) 7_655
C2 C3 1.328(4) .
C3 C4 1.385(5) .
C3 H3 0.9300 .
C4 C5 1.316(5) .
C4 H4 0.9300 .
C5 C4 1.316(5) 7_655
C6 C7 1.410(6) 2_565
C6 C7 1.410(6) .
C7 C8 1.386(7) .
C7 H7 0.9300 .
C8 C9 1.370(6) .
C8 H8 0.9300 .
C9 C10 1.363(12) .
C9 C8 1.370(6) 2_565
C10 N4 1.331(9) 2_565
O1 C11 1.216(10) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 N1 N2 N2 0.1(3) . 7_655
C1 N1 N2 Cu1 -179.4(2) . .
N2 Cu1 N2 N2 -48.51(10) 8 7_655
N2 Cu1 N2 N2 131.49(10) 4_655 7_655
N2 Cu1 N2 N2 100(33) 5_655 7_655
N2 Cu1 N2 N1 130.95(18) 8 .
N2 Cu1 N2 N1 -49.05(18) 4_655 .
N2 Cu1 N2 N1 -81(33) 5_655 .
N3 N3 N4 C10 0.000(6) 2_565 .
N2 N1 C1 N1 -0.2(4) . 7_655
N2 N1 C1 C2 179.5(3) . .
N1 C1 C2 C3 178.3(4) 7_655 7_655
N1 C1 C2 C3 -1.3(7) . 7_655
N1 C1 C2 C3 1.3(7) 7_655 .
N1 C1 C2 C3 -178.3(4) . .
C3 C2 C3 C4 3.3(10) 7_655 .
C1 C2 C3 C4 -179.6(4) . .
C2 C3 C4 C5 0.0(9) . .
C3 C4 C5 C4 -3.4(10) . 7_655
C3 C4 C5 N5 178.5(4) . .
C6 N5 C5 C4 89.1(5) . .
C5 N5 C5 C4 -90.9(5) 2_565 .
C6 N5 C5 C4 -89.1(5) . 7_655
C5 N5 C5 C4 90.9(5) 2_565 7_655
C5 N5 C6 C7 0.000(1) . 2_565
C5 N5 C6 C7 180.000(1) 2_565 2_565
C5 N5 C6 C7 180.000(1) . .
C5 N5 C6 C7 0.000(1) 2_565 .
N5 C6 C7 C8 180.000(1) . .
C7 C6 C7 C8 0.000(2) 2_565 .
C6 C7 C8 C9 0.000(2) . .
C7 C8 C9 C10 180.000(2) . .
C7 C8 C9 C8 0.000(3) . 2_565
N3 N4 C10 N4 0.000(4) . 2_565
N3 N4 C10 C9 180.000(3) . .
C8 C9 C10 N4 0.000(3) . .
C8 C9 C10 N4 180.000(3) 2_565 .
C8 C9 C10 N4 180.000(3) . 2_565
C8 C9 C10 N4 0.000(3) 2_565 2_565
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.043 0.000 0.500 867 206
2 -0.026 0.500 0.000 277 49
