#------------------------------------------------------------------------------
#$Date: 2017-05-04 09:47:45 +0300 (Thu, 04 May 2017) $
#$Revision: 195979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/58/4345806.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_4345806
loop_
_publ_author_name
'Lin, Li-Dan'
'Li, Xin-Xiong'
'Qi, Yan-Jie'
'Ma, Xiang'
'Zheng, Shou-Tian'
_publ_section_title
;
 Cluster Organic Frameworks Constructed from Heterometallic
 Supertetrahedral Cluster Secondary Building Units.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4636
_journal_page_last               4643
_journal_paper_doi               10.1021/acs.inorgchem.7b00267
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C45 H53.5 Cu7 Mn4 N5 O30'
_chemical_formula_weight         1808.96
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   17.1184(8)
_cell_length_b                   17.1184(8)
_cell_length_c                   42.734(2)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.64
_cell_measurement_theta_min      2.35
_cell_volume                     10845.0(9)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            66641
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.672
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             3606
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3596
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0959
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.1448P)²+101.9902P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2778
_refine_ls_wR_factor_ref         0.2921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2658
_reflns_number_total             3596
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00267_si_002.cif
_cod_data_source_block           mo_lld7_54_4_0m
_cod_original_cell_volume        10845.1(12)
_cod_original_formula_sum        'C45 H53.50 Cu7 Mn4 N5 O30'
_cod_database_code               4345806
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.6667 0.3333 0.29673(7) 0.0457(8) Uani 1 6 d S T P
Mn2 Mn 0.79134(7) 0.20866(7) 0.41944(5) 0.0623(6) Uani 1 2 d S T P
Cu1 Cu 0.72846(4) 0.27154(4) 0.35938(3) 0.0395(4) Uani 1 2 d S T P
Cu2 Cu 0.60455(5) 0.20909(10) 0.42050(3) 0.0476(5) Uani 1 2 d S T P
Cu3 Cu 1.3333 0.6667 0.30802(6) 0.0468(7) Uani 1 6 d S T P
C1 C 0.6667 0.3333 0.4853(6) 0.068(3) Uani 1 6 d S TU P
C3 C 1.0488(7) 0.5244(3) 0.3131(2) 0.136(7) Uani 1 2 d DS TU P
H3A H 1.0030 0.5015 0.2983 0.163 Uiso 1 2 calc R U P
C4 C 1.0960(8) 0.5480(4) 0.3665(2) 0.114(5) Uani 1 2 d DS TU P
H4A H 1.0821 0.5411 0.3878 0.137 Uiso 1 2 calc R U P
C5 C 1.1378(7) 0.5689(4) 0.3037(2) 0.125(5) Uani 1 2 d DS TU P
H5A H 1.1519 0.5759 0.2825 0.149 Uiso 1 2 calc R U P
C6 C 0.7171(5) 0.2829(5) 0.4750(3) 0.068(3) Uani 1 2 d S TU P
H6A H 0.7778 0.3139 0.4835 0.082 Uiso 0.5 1 calc R U P
H6B H 0.6861 0.2222 0.4835 0.082 Uiso 0.5 1 calc R U P
C7 C 0.7424(11) 0.485(2) 0.2500 0.108(7) Uani 1 4 d S TU P
C8 C 0.6667 0.3333 0.5220(8) 0.107(5) Uani 1 6 d S TU P
C9 C 0.9269(7) 0.4635(4) 0.3582(2) 0.045(3) Uani 1 2 d S T P
C10 C 0.8654(7) 0.4327(4) 0.3294(3) 0.048(3) Uani 1 2 d S T P
H10A H 0.8790 0.4852 0.3169 0.058 Uiso 0.5 1 calc R U P
H10B H 0.8790 0.3938 0.3169 0.058 Uiso 0.5 1 calc R U P
C11 C 1.0277(6) 0.5138(3) 0.3447(3) 0.064(3) Uani 1 2 d DS TU P
C12 C 0.8290(8) 0.1710(8) 0.3497(5) 0.120(7) Uani 1 2 d S T P
C13 C 0.9145(6) 0.3841(6) 0.3771(2) 0.060(2) Uani 1 1 d . . .
H13A H 0.9265 0.3455 0.3637 0.072 Uiso 1 1 calc R U .
H13B H 0.9587 0.4057 0.3938 0.072 Uiso 1 1 calc R U .
C14 C 1.1851(7) 0.5925(3) 0.3571(2) 0.115(5) Uani 1 2 d DS TU P
H14A H 1.2310 0.6155 0.3719 0.139 Uiso 1 2 calc R U P
C17 C 0.8698(9) 0.1302(9) 0.3311(7) 0.208(17) Uani 1 2 d S T P
H17A H 0.8613 0.1372 0.3093 0.313 Uiso 1 2 calc R U P
H17B H 0.8420 0.0672 0.3361 0.313 Uiso 0.5 1 calc R U P
H17C H 0.9331 0.1592 0.3357 0.313 Uiso 0.5 1 calc R U P
C18 C 0.7973(10) 0.595(2) 0.2500 0.107(5) Uani 1 4 d S TU P
H18A H 0.8060 0.6162 0.2288 0.160 Uiso 0.5 2 calc R U P
H18B H 0.8549 0.6162 0.2598 0.160 Uiso 0.25 1 calc R U P
H18C H 0.7634 0.6162 0.2613 0.160 Uiso 0.25 1 calc R U P
C20 C 0.7029(16) 0.406(3) 0.5762(11) 0.175(10) Uani 0.6667 2 d S TU P
H20A H 0.7302 0.4593 0.5869 0.210 Uiso 0.6667 2 d R U P
C22 C 0.7061(14) 0.412(3) 0.5398(9) 0.142(9) Uani 0.6667 2 d S TU P
H22A H 0.7342 0.4660 0.5301 0.170 Uiso 0.6667 2 d R U P
O1 O 0.8258(4) 0.3309(4) 0.39057(12) 0.0469(13) Uani 1 1 d . . .
O2 O 0.7912(3) 0.2088(3) 0.3352(2) 0.075(3) Uani 1 2 d S T P
O3 O 0.8383(4) 0.1617(4) 0.3822(4) 0.107(4) Uani 1 2 d S T P
O4 O 0.7213(3) 0.2787(3) 0.44159(18) 0.057(2) Uani 1 2 d S T P
O5 O 0.7710(5) 0.3855(2) 0.33659(16) 0.0385(17) Uani 1 2 d S T P
O6 O 0.7295(3) 0.4589(7) 0.2765(2) 0.092(4) Uani 1 2 d S T P
O1W O 0.5448(5) 0.0897(9) 0.4496(3) 0.121(5) Uani 1 2 d S TU P
O2W O 0.7100(7) 0.0900(6) 0.4470(2) 0.112(3) Uani 1 1 d . . .
N1 N 1.2061(5) 0.6030(3) 0.3257(2) 0.062(3) Uani 1 2 d DS TU P
N3 N 0.6667 0.3333 0.5861(6) 0.102(9) Uani 1 6 d S T P
N5 N 1.3333 0.6667 0.2645(4) 0.053(4) Uani 0.5 6 d S T P
C33 N 1.3333 0.6667 0.2645(4) 0.053(4) Uani 0.5 6 d S T P
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'
Mn Mn 0.3368 0.7283 '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
O6 Mn1 O6 103.5(3) 3_665 2_655
O6 Mn1 O6 103.5(3) 3_665 .
O6 Mn1 O6 103.5(3) 2_655 .
O6 Mn1 O5 90.4(2) 3_665 .
O6 Mn1 O5 157.1(3) 2_655 .
O6 Mn1 O5 90.4(2) . .
O6 Mn1 O5 90.4(2) 3_665 3_665
O6 Mn1 O5 90.4(2) 2_655 3_665
O6 Mn1 O5 157.1(3) . 3_665
O5 Mn1 O5 71.2(3) . 3_665
O6 Mn1 O5 157.1(3) 3_665 2_655
O6 Mn1 O5 90.4(2) 2_655 2_655
O6 Mn1 O5 90.4(2) . 2_655
O5 Mn1 O5 71.2(3) . 2_655
O5 Mn1 O5 71.2(3) 3_665 2_655
O3 Mn2 O2W 104.1(3) . 19_665
O3 Mn2 O2W 104.1(3) . .
O2W Mn2 O2W 105.4(5) 19_665 .
O3 Mn2 O1 88.2(3) . 19_665
O2W Mn2 O1 158.1(3) 19_665 19_665
O2W Mn2 O1 88.6(3) . 19_665
O3 Mn2 O1 88.2(3) . .
O2W Mn2 O1 88.6(3) 19_665 .
O2W Mn2 O1 158.1(3) . .
O1 Mn2 O1 73.6(3) 19_665 .
O3 Mn2 O4 155.7(5) . .
O2W Mn2 O4 90.4(3) 19_665 .
O2W Mn2 O4 90.4(3) . .
O1 Mn2 O4 72.5(2) 19_665 .
O1 Mn2 O4 72.5(2) . .
O5 Cu1 O5 85.9(4) 3_665 .
O5 Cu1 O1 91.5(3) 3_665 19_665
O5 Cu1 O1 162.1(2) . 19_665
O5 Cu1 O1 162.1(2) 3_665 .
O5 Cu1 O1 91.5(3) . .
O1 Cu1 O1 85.6(3) 19_665 .
O5 Cu1 O2 103.4(3) 3_665 .
O5 Cu1 O2 103.4(3) . .
O1 Cu1 O2 94.5(3) 19_665 .
O1 Cu1 O2 94.5(3) . .
O1 Cu2 O1 91.0(3) 3_665 19_665
O1 Cu2 O4 161.3(3) 3_665 .
O1 Cu2 O4 85.8(3) 19_665 .
O1 Cu2 O4 85.8(3) 3_665 3_665
O1 Cu2 O4 161.3(3) 19_665 3_665
O4 Cu2 O4 91.4(5) . 3_665
O1 Cu2 O1W 99.1(3) 3_665 .
O1 Cu2 O1W 99.1(3) 19_665 .
O4 Cu2 O1W 99.6(3) . .
O4 Cu2 O1W 99.6(3) 3_665 .
N5 Cu3 N1 111.8(3) . 3_775
N5 Cu3 N1 111.8(3) . 2_755
N1 Cu3 N1 107.0(3) 3_775 2_755
N5 Cu3 N1 111.8(3) . .
N1 Cu3 N1 107.0(3) 3_775 .
N1 Cu3 N1 107.0(3) 2_755 .
C6 C1 C6 112.4(10) 3_665 2_655
C6 C1 C6 112.4(10) 3_665 .
C6 C1 C6 112.4(10) 2_655 .
C6 C1 C8 106.3(11) 3_665 .
C6 C1 C8 106.3(11) 2_655 .
C6 C1 C8 106.4(11) . .
C5 C3 C11 120.1(4) . .
C11 C4 C14 120.3(4) . .
C3 C5 N1 120.2(4) . .
O4 C6 C1 111.4(14) . .
O6 C7 O6 143(3) . 16_556
O6 C7 C18 108.7(16) . .
O6 C7 C18 108.7(16) 16_556 .
C22 C8 C22 93(3) 2_655 .
C22 C8 C22 93(3) 2_655 3_665
C22 C8 C22 93(3) . 3_665
C22 C8 C1 123(2) 2_655 .
C22 C8 C1 123(2) . .
C22 C8 C1 123(2) 3_665 .
C13 C9 C13 113.2(10) . 21
C13 C9 C10 111.0(6) . .
C13 C9 C10 111.0(6) 21 .
C13 C9 C11 107.9(6) . .
C13 C9 C11 108.0(6) 21 .
C10 C9 C11 105.3(9) . .
O5 C10 C9 114.2(9) . .
C4 C11 C3 119.6(4) . .
C4 C11 C9 116.1(8) . .
C3 C11 C9 124.3(8) . .
O2 C12 C17 118(2) . .
O2 C12 O3 129.9(17) . .
C17 C12 O3 112(2) . .
O1 C13 C9 114.4(8) . .
N1 C14 C4 120.1(4) . .
N3 C20 C22 115(5) . .
N3 C20 C20 36.4(17) . 2_655
C22 C20 C20 93(2) . 2_655
N3 C20 C20 36.4(17) . 3_665
C22 C20 C20 93(2) . 3_665
C20 C20 C20 60.001(6) 2_655 3_665
C8 C22 C20 120(4) . .
C8 C22 C22 43.5(15) . 2_655
C20 C22 C22 87(2) . 2_655
C8 C22 C22 43.5(15) . 3_665
C20 C22 C22 87(2) . 3_665
C22 C22 C22 59.999(14) 2_655 3_665
C13 O1 Cu2 115.1(5) . 2_655
C13 O1 Cu1 113.9(5) . .
Cu2 O1 Cu1 108.2(3) 2_655 .
C13 O1 Mn2 120.8(5) . .
Cu2 O1 Mn2 98.9(2) 2_655 .
Cu1 O1 Mn2 97.5(2) . .
C12 O2 Cu1 122.2(11) . .
C12 O3 Mn2 127.6(12) . .
C6 O4 Cu2 115.2(4) . .
C6 O4 Cu2 115.2(4) . 2_655
Cu2 O4 Cu2 108.8(4) . 2_655
C6 O4 Mn2 119.6(8) . .
Cu2 O4 Mn2 97.7(3) . .
Cu2 O4 Mn2 97.7(3) 2_655 .
C10 O5 Cu1 114.8(3) . 2_655
C10 O5 Cu1 114.8(3) . .
Cu1 O5 Cu1 107.7(3) 2_655 .
C10 O5 Mn1 119.9(6) . .
Cu1 O5 Mn1 98.7(2) 2_655 .
Cu1 O5 Mn1 98.7(2) . .
C7 O6 Mn1 133.6(17) . .
C14 N1 C5 119.8(4) . .
C14 N1 Cu3 124.9(6) . .
C5 N1 Cu3 115.3(6) . .
C20 N3 C20 107(3) . 3_665
C20 N3 C20 107(3) . 2_655
C20 N3 C20 107(3) 3_665 2_655
C33 N5 N5 0.000(2) 16_556 16_556
C33 N5 Cu3 180.0 16_556 .
N5 N5 Cu3 180.0 16_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O6 2.053(10) 3_665
Mn1 O6 2.053(10) 2_655
Mn1 O6 2.053(10) .
Mn1 O5 2.301(8) .
Mn1 O5 2.301(8) 3_665
Mn1 O5 2.301(8) 2_655
Mn2 O3 2.113(13) .
Mn2 O2W 2.151(9) 19_665
Mn2 O2W 2.151(9) .
Mn2 O1 2.239(6) 19_665
Mn2 O1 2.239(6) .
Mn2 O4 2.281(9) .
Cu1 O5 1.965(4) 3_665
Cu1 O5 1.965(4) .
Cu1 O1 1.973(5) 19_665
Cu1 O1 1.973(5) .
Cu1 O2 2.127(9) .
Cu2 O1 1.968(5) 3_665
Cu2 O1 1.968(5) 19_665
Cu2 O4 1.961(5) .
Cu2 O4 1.961(5) 3_665
Cu2 O1W 2.164(13) .
Cu3 N5 1.861(17) .
Cu3 N1 2.032(8) 3_775
Cu3 N1 2.032(8) 2_755
Cu3 N1 2.032(8) .
C1 C6 1.557(16) 3_665
C1 C6 1.557(16) 2_655
C1 C6 1.557(16) .
C1 C8 1.57(4) .
C3 C5 1.379(4) .
C3 C11 1.383(4) .
C4 C11 1.379(4) .
C4 C14 1.381(4) .
C5 N1 1.380(4) .
C6 O4 1.435(16) .
C7 O6 1.196(13) .
C7 O6 1.196(13) 16_556
C7 C18 1.63(4) .
C8 C22 1.40(4) 2_655
C8 C22 1.40(4) .
C8 C22 1.40(4) 3_665
C9 C13 1.500(11) .
C9 C13 1.500(11) 21
C9 C10 1.531(15) .
C9 C11 1.602(14) .
C10 O5 1.433(13) .
C12 O2 1.28(2) .
C12 C17 1.45(3) .
C12 O3 1.42(2) .
C13 O1 1.445(10) .
C14 N1 1.377(4) .
C20 N3 1.16(4) .
C20 C22 1.56(6) .
C20 C20 1.86(8) 2_655
C20 C20 1.86(8) 3_665
C22 C22 2.03(7) 2_655
C22 C22 2.03(7) 3_665
O1 Cu2 1.968(5) 2_655
O4 Cu2 1.961(5) 2_655
O5 Cu1 1.965(4) 2_655
N3 C20 1.16(4) 3_665
N3 C20 1.16(5) 2_655
N5 C33 1.24(3) 16_556
N5 N5 1.24(3) 16_556
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 -0.003 -0.002 -0.002 5493.6 440.2
