#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:38:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180190 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/86/7108695.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_7108695
loop_
_publ_author_name
'Lei Zhang'
'Bartosz Marzec'
'Rodolphe Clerac'
'Yanhui Chen'
'Hongzhou Zhang'
'Wolfgang Schmitt'
_publ_section_title
;
 Supramolecular approaches to metal-organic gels using
 ‘Chevrel-type’ coordination clusters as building units
;
_journal_name_full               Chem.Commun.
_journal_page_first              66
_journal_paper_doi               10.1039/c2cc35486a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C62 H100 Cl2 Mn6 N6 O24 P8'
_chemical_formula_weight         1961.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 128.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.109(5)
_cell_length_b                   17.421(3)
_cell_length_c                   14.250(3)
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.22
_cell_volume                     4516(2)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       w-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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13201
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0862
_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)+(0.1284P)²+37.1969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                3161
_reflns_number_total             4094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35486a.txt
_cod_data_source_block           a5
_cod_original_cell_volume        4516.3(24)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7108695
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'
'-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
Mn1 Mn -0.13520(7) 0.5000 -0.50646(12) 0.0220(4) Uani 1 2 d S
Mn2 Mn 0.10109(8) 0.5000 -0.22559(12) 0.0231(4) Uani 1 2 d S
Mn3 Mn 0.0000 0.32653(8) -0.5000 0.0242(4) Uani 1 2 d S
P1 P -0.02321(10) 0.37861(9) -0.31429(15) 0.0223(4) Uani 1 1 d .
P2 P -0.16344(10) 0.37850(11) -0.69288(16) 0.0295(5) Uani 1 1 d .
O1 O -0.0901(3) 0.4249(4) -0.3903(6) 0.064(2) Uani 1 1 d .
O2 O 0.0414(4) 0.4267(4) -0.2320(5) 0.063(2) Uani 1 1 d .
O3 O -0.0130(5) 0.3272(3) -0.3851(6) 0.069(2) Uani 1 1 d .
O4 O -0.1768(3) 0.4254(4) -0.6218(6) 0.071(2) Uani 1 1 d .
O5 O -0.0994(3) 0.3274(3) -0.6189(7) 0.072(2) Uani 1 1 d .
O6 O -0.1572(4) 0.4255(4) -0.7737(5) 0.068(2) Uani 1 1 d .
N1 N -0.2324(4) 0.5000 -0.5107(7) 0.033(2) Uani 1 2 d S
N2 N 0.1723(5) 0.5000 -0.0304(7) 0.039(2) Uani 1 2 d S
N3 N 0.0000 0.1998(5) -0.5000 0.036(2) Uani 1 2 d S
C1 C -0.0342(5) 0.3177(4) -0.2229(7) 0.0390(19) Uani 1 1 d .
C2 C -0.2416(5) 0.3155(6) -0.7829(8) 0.056(3) Uani 1 1 d .
C3 C 0.292(2) 0.5000 0.158(3) 0.187(14) Uani 1 2 d SU
H3A H 0.3426 0.5000 0.2019 0.225 Uiso 1 2 calc SR
C12 C -0.0293(6) 0.1607(5) -0.5976(8) 0.059(3) Uani 1 1 d .
H12A H -0.0516 0.1874 -0.6687 0.071 Uiso 1 1 calc R
C13 C 0.0000 0.0427(5) -0.5000 0.033(2) Uani 1 2 d SU
C14 C -0.0936(6) 0.2597(6) -0.3052(10) 0.070(3) Uani 1 1 d .
H14A H -0.1012 0.2266 -0.2598 0.106 Uiso 1 1 calc R
H14B H -0.0787 0.2296 -0.3434 0.106 Uiso 1 1 calc R
H14C H -0.1385 0.2861 -0.3645 0.106 Uiso 1 1 calc R
C15 C -0.0588(6) 0.3688(6) -0.1668(9) 0.059(3) Uani 1 1 d .
H15A H -0.0656 0.3382 -0.1183 0.089 Uiso 1 1 calc R
H15B H -0.1043 0.3933 -0.2284 0.089 Uiso 1 1 calc R
H15C H -0.0220 0.4071 -0.1183 0.089 Uiso 1 1 calc R
C16 C -0.0290(7) 0.0836(5) -0.6005(9) 0.064(3) Uani 1 1 d .
H16A H -0.0488 0.0584 -0.6720 0.077 Uiso 1 1 calc R
C18 C -0.2650(6) 0.4386(7) -0.5192(11) 0.073(3) Uani 1 1 d .
H18A H -0.2435 0.3929 -0.5172 0.088 Uiso 1 1 calc R
C19 C 0.0356(6) 0.2788(6) -0.1313(9) 0.063(3) Uani 1 1 d .
H19A H 0.0293 0.2467 -0.0835 0.094 Uiso 1 1 calc R
H19B H 0.0729 0.3164 -0.0815 0.094 Uiso 1 1 calc R
H19C H 0.0502 0.2479 -0.1693 0.094 Uiso 1 1 calc R
C23 C -0.2443(7) 0.2630(8) -0.7049(11) 0.101(5) Uani 1 1 d .
H23A H -0.2860 0.2295 -0.7527 0.152 Uiso 1 1 calc R
H23B H -0.2487 0.2922 -0.6524 0.152 Uiso 1 1 calc R
H23C H -0.2001 0.2330 -0.6587 0.152 Uiso 1 1 calc R
C30 C 0.1458(9) 0.5000 0.0295(11) 0.071(4) Uani 1 2 d S
H30A H 0.0951 0.5000 -0.0136 0.085 Uiso 1 2 calc SR
C31 C 0.1883(13) 0.5000 0.1495(16) 0.102(7) Uani 1 2 d S
H31A H 0.1670 0.5000 0.1876 0.123 Uiso 1 2 calc SR
C32 C 0.2575(12) 0.5000 0.2096(15) 0.152(13) Uani 1 2 d S
H32A H 0.2865 0.5000 0.2923 0.183 Uiso 1 2 calc SR
C33 C 0.2409(14) 0.5000 0.027(2) 0.125(8) Uani 1 2 d SU
H33A H 0.2599 0.5000 -0.0151 0.149 Uiso 1 2 calc SR
C34 C -0.3279(7) 0.4323(10) -0.5310(14) 0.110(6) Uani 1 1 d .
H34A H -0.3467 0.3853 -0.5303 0.132 Uiso 1 1 calc R
C35 C -0.3610(10) 0.5000 -0.544(2) 0.124(9) Uani 1 2 d S
H35A H -0.4071 0.5000 -0.5619 0.148 Uiso 1 2 calc SR
C36 C -0.2335(7) 0.2741(9) -0.8643(12) 0.112(6) Uani 1 1 d .
H36A H -0.2743 0.2398 -0.9134 0.169 Uiso 1 1 calc R
H36B H -0.1886 0.2452 -0.8187 0.169 Uiso 1 1 calc R
H36C H -0.2323 0.3103 -0.9140 0.169 Uiso 1 1 calc R
C37 C -0.3086(6) 0.3634(9) -0.8498(14) 0.134(7) Uani 1 1 d .
H37A H -0.3511 0.3311 -0.8983 0.201 Uiso 1 1 calc R
H37B H -0.3069 0.3986 -0.8999 0.201 Uiso 1 1 calc R
H37C H -0.3114 0.3916 -0.7949 0.201 Uiso 1 1 calc R
Cl1 Cl -0.5000 0.0000 -0.5000 0.0233(7) Uani 1 4 d S
Cl2 Cl -0.0458(14) 0.0000 -0.840(2) 0.243(11) Uiso 0.50 2 d SP
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'
Cl Cl 0.1484 0.1585 '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'
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'
P P 0.1023 0.0942 '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
O4 Mn1 O4 90.2(6) . 6_565
O4 Mn1 O1 177.7(3) . 6_565
O4 Mn1 O1 89.7(4) 6_565 6_565
O4 Mn1 O1 89.7(4) . .
O4 Mn1 O1 177.7(3) 6_565 .
O1 Mn1 O1 90.2(5) 6_565 .
O4 Mn1 N1 90.8(2) . .
O4 Mn1 N1 90.8(2) 6_565 .
O1 Mn1 N1 91.5(2) 6_565 .
O1 Mn1 N1 91.5(2) . .
O6 Mn2 O6 89.8(5) 5_564 2_554
O6 Mn2 O2 177.4(3) 5_564 .
O6 Mn2 O2 91.2(4) 2_554 .
O6 Mn2 O2 91.2(4) 5_564 6_565
O6 Mn2 O2 177.4(3) 2_554 6_565
O2 Mn2 O2 87.8(5) . 6_565
O6 Mn2 N2 91.5(3) 5_564 .
O6 Mn2 N2 91.5(3) 2_554 .
O2 Mn2 N2 90.9(2) . .
O2 Mn2 N2 90.9(2) 6_565 .
O5 Mn3 O5 179.1(4) . 2_554
O5 Mn3 O3 91.3(4) . .
O5 Mn3 O3 88.7(4) 2_554 .
O5 Mn3 O3 88.7(4) . 2_554
O5 Mn3 O3 91.3(4) 2_554 2_554
O3 Mn3 O3 179.3(3) . 2_554
O5 Mn3 N3 90.45(18) . .
O5 Mn3 N3 90.45(18) 2_554 .
O3 Mn3 N3 90.34(16) . .
O3 Mn3 N3 90.34(16) 2_554 .
O2 P1 O1 111.5(4) . .
O2 P1 O3 112.5(5) . .
O1 P1 O3 111.7(4) . .
O2 P1 C1 106.5(3) . .
O1 P1 C1 107.5(3) . .
O3 P1 C1 106.8(3) . .
O5 P2 O4 112.7(5) . .
O5 P2 O6 110.7(5) . .
O4 P2 O6 112.8(5) . .
O5 P2 C2 105.3(4) . .
O4 P2 C2 106.5(4) . .
O6 P2 C2 108.4(4) . .
P1 O1 Mn1 143.8(4) . .
P1 O2 Mn2 143.0(3) . .
P1 O3 Mn3 142.8(3) . .
P2 O4 Mn1 142.4(4) . .
P2 O5 Mn3 143.2(4) . .
P2 O6 Mn2 142.7(3) . 5_564
C18 N1 C18 114.7(12) . 6_565
C18 N1 Mn1 122.4(6) . .
C18 N1 Mn1 122.4(6) 6_565 .
C33 N2 C30 119.0(15) . .
C33 N2 Mn2 118.7(13) . .
C30 N2 Mn2 122.4(8) . .
C12 N3 C12 116.9(9) . 2_554
C12 N3 Mn3 121.5(5) . .
C12 N3 Mn3 121.5(5) 2_554 .
C19 C1 C14 110.7(8) . .
C19 C1 C15 111.4(8) . .
C14 C1 C15 110.1(8) . .
C19 C1 P1 110.0(6) . .
C14 C1 P1 107.2(6) . .
C15 C1 P1 107.4(5) . .
C23 C2 C36 112.1(11) . .
C23 C2 C37 108.9(12) . .
C36 C2 C37 111.1(11) . .
C23 C2 P2 109.4(7) . .
C36 C2 P2 107.4(7) . .
C37 C2 P2 107.9(8) . .
C32 C3 C33 114(3) . .
C32 C3 H3A 122.9 . .
C33 C3 H3A 122.9 . .
N3 C12 C16 123.2(9) . .
N3 C12 H12A 118.4 . .
C16 C12 H12A 118.4 . .
C16 C13 C16 116.3(10) 2_554 .
C16 C13 C13 121.9(5) 2_554 5_554
C16 C13 C13 121.9(5) . 5_554
C1 C14 H14A 109.5 . .
C1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C1 C15 H15A 109.5 . .
C1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C12 C16 C13 120.2(9) . .
C12 C16 H16A 119.9 . .
C13 C16 H16A 119.9 . .
N1 C18 C34 127.2(12) . .
N1 C18 H18A 116.4 . .
C34 C18 H18A 116.4 . .
C1 C19 H19A 109.5 . .
C1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C2 C23 H23A 109.5 . .
C2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N2 C30 C31 123.7(17) . .
N2 C30 H30A 118.2 . .
C31 C30 H30A 118.2 . .
C32 C31 C30 119(2) . .
C32 C31 H31A 120.5 . .
C30 C31 H31A 120.5 . .
C31 C32 C3 123(2) . .
C31 C32 H32A 118.6 . .
C3 C32 H32A 118.6 . .
N2 C33 C3 121(2) . .
N2 C33 H33A 119.4 . .
C3 C33 H33A 119.4 . .
C35 C34 C18 114.6(15) . .
C35 C34 H34A 122.7 . .
C18 C34 H34A 122.7 . .
C34 C35 C34 121.1(17) 6_565 .
C34 C35 H35A 119.5 6_565 .
C34 C35 H35A 119.5 . .
C2 C36 H36A 109.5 . .
C2 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C2 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C2 C37 H37A 109.5 . .
C2 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C2 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 1.835(5) .
Mn1 O4 1.835(5) 6_565
Mn1 O1 1.847(6) 6_565
Mn1 O1 1.847(6) .
Mn1 N1 2.209(8) .
Mn2 O6 1.840(6) 5_564
Mn2 O6 1.840(6) 2_554
Mn2 O2 1.840(5) .
Mn2 O2 1.840(5) 6_565
Mn2 N2 2.191(8) .
Mn3 O5 1.830(6) .
Mn3 O5 1.830(6) 2_554
Mn3 O3 1.838(5) .
Mn3 O3 1.838(5) 2_554
Mn3 N3 2.207(8) .
P1 O2 1.465(6) .
P1 O1 1.466(6) .
P1 O3 1.473(5) .
P1 C1 1.815(7) .
P2 O5 1.473(7) .
P2 O4 1.474(6) .
P2 O6 1.490(6) .
P2 C2 1.804(8) .
O6 Mn2 1.840(6) 5_564
N1 C18 1.270(11) .
N1 C18 1.270(11) 6_565
N2 C33 1.26(3) .
N2 C30 1.321(18) .
N3 C12 1.302(10) .
N3 C12 1.302(10) 2_554
C1 C19 1.474(12) .
C1 C14 1.515(12) .
C1 C15 1.520(12) .
C2 C23 1.470(15) .
C2 C36 1.474(14) .
C2 C37 1.477(17) .
C3 C32 1.37(4) .
C3 C33 1.47(4) .
C3 H3A 0.9300 .
C12 C16 1.344(12) .
C12 H12A 0.9300 .
C13 C16 1.352(10) 2_554
C13 C16 1.352(10) .
C13 C13 1.487(19) 5_554
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9300 .
C18 C34 1.361(14) .
C18 H18A 0.9300 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C30 C31 1.35(2) .
C30 H30A 0.9300 .
C31 C32 1.27(3) .
C31 H31A 0.9300 .
C32 H32A 0.9300 .
C33 H33A 0.9300 .
C34 C35 1.355(17) .
C34 H34A 0.9300 .
C35 C34 1.355(17) 6_565
C35 H35A 0.9300 .
C36 H36A 0.9600 .
C36 H36B 0.9600 .
C36 H36C 0.9600 .
C37 H37A 0.9600 .
C37 H37B 0.9600 .
C37 H37C 0.9600 .
