#------------------------------------------------------------------------------
#$Date: 2019-11-23 22:18:16 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235331 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/62/7236267.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_7236267
loop_
_publ_author_name
'Gong, Chunhua'
'Zeng, Xianghua'
'Zhu, Chengfeng'
'Shu, Jiahui'
'Xiao, Pingxiu'
'Xu, Hao'
'Liu, Lichun'
'Zhang, Junyong'
'Zeng, Qingdao'
'Xie, Jingli'
_publ_section_title
;
 A series of organic--inorganic hybrid materials consisting of flexible
 organic amine modified polyoxomolybdates: synthesis, structures and
 properties
;
_journal_issue                   108
_journal_name_full               'RSC Advances'
_journal_page_first              106248
_journal_paper_doi               10.1039/C6RA21603J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C36 H36 Cu2 Mo8 N8 O26'
_chemical_formula_weight         1891.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-12 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8760(3)
_cell_length_b                   15.9080(3)
_cell_length_c                   18.9788(3)
_cell_measurement_reflns_used    5733
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.9270
_cell_measurement_theta_min      2.9100
_cell_volume                     5095.11(15)
_computing_cell_refinement
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_data_collection
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_data_reduction
;

CrysAlisPro, Agilent Technologies,

Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)

(compiled Aug 13 2014,18:06:01)

;
_computing_molecular_graphics    SHELXL-2014
_computing_publication_material  SHELXL-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXL-2014/
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         2.732
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93189
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.466
_exptl_crystal_description       block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0198P)²+3.7988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4861
_reflns_number_total             5920
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra21603j2.cif
_cod_data_source_block           6
_cod_original_cell_volume        5095.10(15)
_cod_database_code               7236267
_shelx_shelxl_version_number     2014/7
_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.

;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo1 Mo 0.17951(2) 0.62807(2) 0.48371(2) 0.02088(7) Uani 1 1 d . .
Mo2 Mo -0.03493(2) 0.46838(2) 0.41507(2) 0.01725(7) Uani 1 1 d . .
Mo3 Mo 0.14535(2) 0.42657(2) 0.45108(2) 0.02099(7) Uani 1 1 d . .
Mo4 Mo -0.00593(2) 0.66618(2) 0.43973(2) 0.02110(7) Uani 1 1 d . .
Cu1 Cu 0.24855(2) 0.70133(3) 0.31278(2) 0.02180(10) Uani 1 1 d . .
O7 O 0.03667(13) 0.37934(14) 0.44524(11) 0.0207(5) Uani 1 1 d . .
O10 O -0.08702(13) 0.57556(14) 0.43261(11) 0.0209(5) Uani 1 1 d . .
O3 O 0.09008(13) 0.70179(14) 0.48500(11) 0.0240(5) Uani 1 1 d . .
O13 O 0.05980(12) 0.53872(13) 0.46051(11) 0.0182(5) Uani 1 1 d . .
O9 O -0.01029(14) 0.47787(15) 0.32917(12) 0.0278(6) Uani 1 1 d . .
O4 O 0.21127(13) 0.51435(14) 0.48956(11) 0.0235(5) Uani 1 1 d . .
O1 O 0.20639(14) 0.64680(15) 0.39550(11) 0.0276(5) Uani 1 1 d . .
O6 O 0.19820(15) 0.34147(16) 0.47705(13) 0.0342(6) Uani 1 1 d . .
O5 O 0.16379(15) 0.43556(16) 0.36337(12) 0.0311(6) Uani 1 1 d . .
O2 O 0.24944(15) 0.67833(17) 0.53110(13) 0.0351(6) Uani 1 1 d . .
O8 O -0.12208(13) 0.40746(15) 0.41481(11) 0.0245(5) Uani 1 1 d . .
O12 O 0.02122(15) 0.66920(15) 0.35326(12) 0.0318(6) Uani 1 1 d . .
N3 N 0.18922(16) 0.81641(17) 0.31779(14) 0.0236(6) Uani 1 1 d . .
N1 N 0.19841(16) 0.62096(18) 0.24083(14) 0.0232(6) Uani 1 1 d . .
O11 O -0.06458(15) 0.75183(15) 0.44934(13) 0.0337(6) Uani 1 1 d . .
N4 N 0.29347(16) 0.75301(17) 0.22307(14) 0.0229(6) Uani 1 1 d . .
N2 N 0.36477(17) 0.70521(18) 0.34340(15) 0.0270(7) Uani 1 1 d . .
C17 C 0.19712(19) 0.8616(2) 0.25843(17) 0.0225(7) Uani 1 1 d . .
C7 C 0.3966(2) 0.6685(2) 0.40057(19) 0.0322(8) Uani 1 1 d . .
H7 H 0.3634 0.6423 0.4329 0.039 Uiso 1 1 calc R U
C5 C 0.2329(2) 0.6243(2) 0.17683(17) 0.0247(8) Uani 1 1 d . .
C6 C 0.3025(2) 0.6834(2) 0.17120(18) 0.0278(8) Uani 1 1 d . .
H6A H 0.3513 0.6531 0.1804 0.033 Uiso 1 1 calc R U
H6B H 0.3053 0.7063 0.1239 0.033 Uiso 1 1 calc R U
C18 C 0.2355(2) 0.8167(2) 0.19770(17) 0.0276(8) Uani 1 1 d . .
H18A H 0.1950 0.7891 0.1697 0.033 Uiso 1 1 calc R U
H18B H 0.2624 0.8572 0.1679 0.033 Uiso 1 1 calc R U
C11 C 0.4127(2) 0.7449(2) 0.29762(18) 0.0267(8) Uani 1 1 d . .
C12 C 0.3712(2) 0.7922(2) 0.24006(19) 0.0294(8) Uani 1 1 d . .
H12A H 0.3629 0.8499 0.2548 0.035 Uiso 1 1 calc R U
H12B H 0.4041 0.7927 0.1982 0.035 Uiso 1 1 calc R U
C4 C 0.2075(2) 0.5744(2) 0.12149(19) 0.0343(9) Uani 1 1 d . .
H4 H 0.2318 0.5779 0.0776 0.041 Uiso 1 1 calc R U
C1 C 0.1371(2) 0.5684(2) 0.25076(18) 0.0283(8) Uani 1 1 d . .
H1 H 0.1126 0.5666 0.2946 0.034 Uiso 1 1 calc R U
C16 C 0.1675(2) 0.9423(2) 0.25216(19) 0.0294(8) Uani 1 1 d . .
H16 H 0.1743 0.9728 0.2108 0.035 Uiso 1 1 calc R U
C13 C 0.1512(2) 0.8508(2) 0.37260(19) 0.0323(9) Uani 1 1 d . .
H13 H 0.1459 0.8199 0.4140 0.039 Uiso 1 1 calc R U
C2 C 0.1096(2) 0.5168(2) 0.1975(2) 0.0336(9) Uani 1 1 d . .
H2 H 0.0671 0.4808 0.2055 0.040 Uiso 1 1 calc R U
C3 C 0.1456(2) 0.5193(3) 0.1326(2) 0.0400(10) Uani 1 1 d . .
H3 H 0.1284 0.4842 0.0965 0.048 Uiso 1 1 calc R U
C10 C 0.4940(2) 0.7470(3) 0.3064(2) 0.0380(10) Uani 1 1 d . .
H10 H 0.5262 0.7737 0.2735 0.046 Uiso 1 1 calc R U
C15 C 0.1276(3) 0.9767(2) 0.3085(2) 0.0437(11) Uani 1 1 d . .
H15 H 0.1062 1.0304 0.3053 0.052 Uiso 1 1 calc R U
C8 C 0.4776(2) 0.6685(3) 0.4125(2) 0.0381(10) Uani 1 1 d . .
H8 H 0.4986 0.6420 0.4520 0.046 Uiso 1 1 calc R U
C14 C 0.1197(3) 0.9307(3) 0.3693(2) 0.0449(11) Uani 1 1 d . .
H14 H 0.0934 0.9533 0.4080 0.054 Uiso 1 1 calc R U
C9 C 0.5265(2) 0.7084(3) 0.3649(2) 0.0418(10) Uani 1 1 d . .
H9 H 0.5810 0.7095 0.3722 0.050 Uiso 1 1 calc R U
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
O2 Mo1 O1 104.29(11) . .
O2 Mo1 O4 102.95(12) . .
O1 Mo1 O4 98.32(10) . .
O2 Mo1 O3 104.77(12) . .
O1 Mo1 O3 96.43(10) . .
O4 Mo1 O3 144.14(10) . .
O2 Mo1 O8 87.92(10) . 5_566
O1 Mo1 O8 167.68(10) . 5_566
O4 Mo1 O8 80.20(9) . 5_566
O3 Mo1 O8 78.53(9) . 5_566
O2 Mo1 O13 157.84(9) . .
O1 Mo1 O13 97.85(9) . .
O4 Mo1 O13 72.33(8) . .
O3 Mo1 O13 73.39(8) . .
O8 Mo1 O13 69.99(7) 5_566 .
O9 Mo2 O8 104.60(10) . .
O9 Mo2 O10 101.42(10) . .
O8 Mo2 O10 96.04(10) . .
O9 Mo2 O7 101.30(11) . .
O8 Mo2 O7 96.81(10) . .
O10 Mo2 O7 150.07(9) . .
O9 Mo2 O13 99.14(10) . .
O8 Mo2 O13 156.26(9) . .
O10 Mo2 O13 79.04(9) . .
O7 Mo2 O13 78.33(9) . .
O9 Mo2 O13 175.13(9) . 5_566
O8 Mo2 O13 80.26(9) . 5_566
O10 Mo2 O13 78.12(8) . 5_566
O7 Mo2 O13 77.59(8) . 5_566
O13 Mo2 O13 76.00(8) . 5_566
O9 Mo2 Mo3 89.46(8) . .
O8 Mo2 Mo3 133.05(8) . .
O10 Mo2 Mo3 125.23(6) . .
O7 Mo2 Mo3 36.23(6) . .
O13 Mo2 Mo3 46.19(6) . .
O13 Mo2 Mo3 86.91(5) 5_566 .
O9 Mo2 Mo4 90.89(8) . .
O8 Mo2 Mo4 131.70(8) . .
O10 Mo2 Mo4 35.67(6) . .
O7 Mo2 Mo4 125.02(6) . .
O13 Mo2 Mo4 46.73(6) . .
O13 Mo2 Mo4 85.96(5) 5_566 .
Mo3 Mo2 Mo4 91.586(10) . .
O6 Mo3 O5 104.82(12) . .
O6 Mo3 O4 99.48(11) . .
O5 Mo3 O4 101.79(11) . .
O6 Mo3 O7 101.55(11) . .
O5 Mo3 O7 98.42(11) . .
O4 Mo3 O7 145.89(9) . .
O6 Mo3 O13 157.92(10) . .
O5 Mo3 O13 97.23(10) . .
O4 Mo3 O13 76.77(8) . .
O7 Mo3 O13 73.63(8) . .
O6 Mo3 O10 86.42(10) . 5_566
O5 Mo3 O10 165.98(10) . 5_566
O4 Mo3 O10 84.22(8) . 5_566
O7 Mo3 O10 70.69(8) . 5_566
O13 Mo3 O10 71.60(7) . 5_566
O6 Mo3 Mo2 136.99(9) . .
O5 Mo3 Mo2 86.97(9) . .
O4 Mo3 Mo2 118.71(7) . .
O7 Mo3 Mo2 35.45(6) . .
O13 Mo3 Mo2 41.98(5) . .
O10 Mo3 Mo2 79.05(5) 5_566 .
O11 Mo4 O12 103.78(12) . .
O11 Mo4 O3 101.99(11) . .
O12 Mo4 O3 101.28(11) . .
O11 Mo4 O10 100.84(11) . .
O12 Mo4 O10 98.03(10) . .
O3 Mo4 O10 145.46(9) . .
O11 Mo4 O13 162.54(10) . .
O12 Mo4 O13 93.38(10) . .
O3 Mo4 O13 77.32(8) . .
O10 Mo4 O13 73.18(8) . .
O11 Mo4 O7 91.08(10) . 5_566
O12 Mo4 O7 163.58(10) . 5_566
O3 Mo4 O7 82.06(8) . 5_566
O10 Mo4 O7 71.91(8) . 5_566
O13 Mo4 O7 71.51(7) . 5_566
O11 Mo4 Mo2 135.49(9) . .
O12 Mo4 Mo2 85.89(8) . .
O3 Mo4 Mo2 118.81(7) . .
O10 Mo4 Mo2 34.74(6) . .
O13 Mo4 Mo2 41.49(5) . .
O7 Mo4 Mo2 78.52(5) 5_566 .
O1 Cu1 N4 177.07(11) . .
O1 Cu1 N2 97.81(11) . .
N4 Cu1 N2 82.44(11) . .
O1 Cu1 N1 96.27(10) . .
N4 Cu1 N1 81.31(11) . .
N2 Cu1 N1 127.06(11) . .
O1 Cu1 N3 100.38(10) . .
N4 Cu1 N3 82.11(11) . .
N2 Cu1 N3 114.83(11) . .
N1 Cu1 N3 112.24(11) . .
Mo2 O7 Mo3 108.32(10) . .
Mo2 O7 Mo4 111.05(10) . 5_566
Mo3 O7 Mo4 105.53(9) . 5_566
Mo2 O10 Mo4 109.58(10) . .
Mo2 O10 Mo3 109.13(9) . 5_566
Mo4 O10 Mo3 103.17(9) . 5_566
Mo1 O3 Mo4 118.66(11) . .
Mo2 O13 Mo3 91.84(8) . .
Mo2 O13 Mo4 91.78(8) . .
Mo3 O13 Mo4 162.53(10) . .
Mo2 O13 Mo2 104.00(8) . 5_566
Mo3 O13 Mo2 98.61(8) . 5_566
Mo4 O13 Mo2 97.09(8) . 5_566
Mo2 O13 Mo1 166.26(10) . .
Mo3 O13 Mo1 87.01(7) . .
Mo4 O13 Mo1 85.44(7) . .
Mo2 O13 Mo1 89.71(7) 5_566 .
Mo1 O4 Mo3 120.47(11) . .
Mo1 O1 Cu1 160.93(15) . .
Mo2 O8 Mo1 120.02(11) . 5_566
C13 N3 C17 118.8(3) . .
C13 N3 Cu1 128.5(2) . .
C17 N3 Cu1 112.5(2) . .
C1 N1 C5 118.9(3) . .
C1 N1 Cu1 127.7(2) . .
C5 N1 Cu1 113.4(2) . .
C12 N4 C18 111.4(3) . .
C12 N4 C6 111.4(3) . .
C18 N4 C6 111.0(3) . .
C12 N4 Cu1 108.4(2) . .
C18 N4 Cu1 107.5(2) . .
C6 N4 Cu1 106.89(19) . .
C11 N2 C7 119.0(3) . .
C11 N2 Cu1 114.0(2) . .
C7 N2 Cu1 126.8(3) . .
N3 C17 C16 122.2(3) . .
N3 C17 C18 115.6(3) . .
C16 C17 C18 122.1(3) . .
N2 C7 C8 121.8(4) . .
N1 C5 C4 121.8(3) . .
N1 C5 C6 115.1(3) . .
C4 C5 C6 123.0(3) . .
N4 C6 C5 109.7(3) . .
N4 C18 C17 111.0(3) . .
N2 C11 C10 122.1(3) . .
N2 C11 C12 115.1(3) . .
C10 C11 C12 122.6(3) . .
N4 C12 C11 111.1(3) . .
C3 C4 C5 118.9(3) . .
N1 C1 C2 121.7(3) . .
C15 C16 C17 118.6(3) . .
N3 C13 C14 121.7(4) . .
C3 C2 C1 119.3(4) . .
C2 C3 C4 119.3(4) . .
C11 C10 C9 118.6(4) . .
C14 C15 C16 119.3(4) . .
C9 C8 C7 118.9(4) . .
C15 C14 C13 119.4(4) . .
C8 C9 C10 119.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.686(2) .
Mo1 O1 1.760(2) .
Mo1 O4 1.890(2) .
Mo1 O3 1.911(2) .
Mo1 O8 2.229(2) 5_566
Mo1 O13 2.509(2) .
Mo2 O9 1.689(2) .
Mo2 O8 1.761(2) .
Mo2 O10 1.947(2) .
Mo2 O7 1.948(2) .
Mo2 O13 2.134(2) .
Mo2 O13 2.401(2) 5_566
Mo2 Mo3 3.1885(4) .
Mo2 Mo4 3.2187(4) .
Mo3 O6 1.694(2) .
Mo3 O5 1.699(2) .
Mo3 O4 1.929(2) .
Mo3 O7 1.985(2) .
Mo3 O13 2.302(2) .
Mo3 O10 2.417(2) 5_566
Mo4 O11 1.694(2) .
Mo4 O12 1.705(2) .
Mo4 O3 1.920(2) .
Mo4 O10 1.992(2) .
Mo4 O13 2.345(2) .
Mo4 O7 2.358(2) 5_566
Cu1 O1 1.930(2) .
Cu1 N4 2.037(3) .
Cu1 N2 2.047(3) .
Cu1 N1 2.053(3) .
Cu1 N3 2.089(3) .
O7 Mo4 2.358(2) 5_566
O10 Mo3 2.417(2) 5_566
O13 Mo2 2.401(2) 5_566
O8 Mo1 2.229(2) 5_566
N3 C13 1.339(4) .
N3 C17 1.343(4) .
N1 C1 1.344(4) .
N1 C5 1.348(4) .
N4 C12 1.487(4) .
N4 C18 1.489(4) .
N4 C6 1.489(4) .
N2 C11 1.345(4) .
N2 C7 1.345(4) .
C17 C16 1.384(5) .
C17 C18 1.502(5) .
C7 C8 1.385(5) .
C5 C4 1.385(5) .
C5 C6 1.508(5) .
C11 C10 1.383(5) .
C11 C12 1.500(5) .
C4 C3 1.380(5) .
C1 C2 1.383(5) .
C16 C15 1.376(5) .
C13 C14 1.380(5) .
C2 C3 1.374(5) .
C10 C9 1.383(5) .
C15 C14 1.373(6) .
C8 C9 1.379(6) .
