#------------------------------------------------------------------------------
#$Date: 2019-11-07 20:37:41 +0100 (jue 07 de nov de 2019) $
#$Revision: 223563 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/42/7234234.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_7234234
loop_
_publ_author_name
'Pan, Xiang'
'Wang, Xiuli'
'Wang, Xiang'
'Li, Yan'
'Liu, Guocheng'
'Lin, Hongyan'
_publ_section_title
;
 Various types of isopolymolybdate-based metal--organic complexes formed
 in different conditions: synthesis, structures, luminescence,
 electrochemical, and photocatalytic performances
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6472
_journal_paper_doi               10.1039/C9CE01394F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C7 H10 Mo3 N3 Ni O15'
_chemical_formula_weight         722.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-13 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                109.5950(10)
_cell_angle_beta                 94.9980(10)
_cell_angle_gamma                105.4480(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0455(3)
_cell_length_b                   10.2229(4)
_cell_length_c                   12.4994(5)
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.267
_cell_measurement_theta_min      1.763
_cell_volume                     915.73(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.267
_diffrn_reflns_theta_min         1.763
_exptl_absorpt_coefficient_mu    3.102
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.727
_exptl_transmission_factor_min   0.653
_refine_diff_density_max         0.850
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0253
_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)+(0.0370P)²+1.7789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4044
_reflns_number_total             4504
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01394f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7234233--7234237.cif.'
_cod_database_code               7234234
_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.
;
_shelx_estimated_absorpt_t_min   0.653
_shelx_estimated_absorpt_t_max   0.727
loop_
_space_group_symop_operation_xyz
'x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ni1 Ni 0.14000(6) -0.24094(5) 0.72098(4) 0.01448(10) Uani 1 1 d . .
C1 C 0.4329(5) -0.3868(4) 1.0053(3) 0.0191(7) Uani 1 1 d . .
O1 O 0.2801(4) -0.3071(3) 0.8286(2) 0.0216(5) Uani 1 1 d . .
N1 N 0.1825(4) -0.0726(3) 0.8778(3) 0.0187(6) Uani 1 1 d . .
O1W O -0.4226(6) -0.3518(6) 0.6896(5) 0.0841(16) Uani 1 1 d . .
H1WA H -0.3229 -0.2984 0.7322 0.101 Uiso 1 1 d R U
H1WB H -0.4771 -0.2956 0.6782 0.101 Uiso 1 1 d R U
Mo1 Mo 0.44132(3) -0.00708(3) 0.61736(2) 0.01095(7) Uani 1 1 d . .
Mo2 Mo 0.15578(3) -0.17635(3) 0.30716(2) 0.01199(7) Uani 1 1 d . .
C2 C 0.5479(6) -0.3760(4) 1.0990(3) 0.0294(9) Uani 1 1 d . .
H2B H 0.5798 -0.2898 1.1683 0.035 Uiso 1 1 d R U
N2 N 0.1606(4) 0.0578(3) 0.9221(3) 0.0210(6) Uani 1 1 d . .
H2A H 0.1112 0.0988 0.8801 0.025 Uiso 1 1 d R U
O2 O -0.0054(3) -0.1695(3) 0.6239(2) 0.0208(5) Uani 1 1 d . .
O2W O 0.3814(7) -0.4078(7) 0.4556(6) 0.1005(19) Uani 1 1 d . .
H2WA H 0.2879 -0.4190 0.4830 0.121 Uiso 1 1 d R U
H2WB H 0.4157 -0.3205 0.4580 0.121 Uiso 1 1 d R U
Mo3 Mo -0.14170(3) -0.14549(3) 0.52191(2) 0.01188(7) Uani 1 1 d . .
O3 O -0.2544(4) -0.3192(3) 0.4284(2) 0.0256(6) Uani 1 1 d . .
N3 N 0.3708(4) -0.2658(3) 1.0182(3) 0.0202(6) Uani 1 1 d . .
H3A H 0.3775 -0.2057 1.0911 0.024 Uiso 1 1 d R U
C3 C 0.6163(6) -0.4884(4) 1.0943(3) 0.0296(9) Uani 1 1 d . .
H3B H 0.6925 -0.4623 1.1667 0.044 Uiso 1 1 d R U
O4 O -0.2980(3) -0.0785(3) 0.6053(2) 0.0161(5) Uani 1 1 d . .
C4 C 0.3040(5) -0.2317(4) 0.9337(3) 0.0175(7) Uani 1 1 d . .
O5 O 0.0395(3) -0.0953(2) 0.4290(2) 0.0137(4) Uani 1 1 d . .
C5 C 0.2609(4) -0.0937(4) 0.9665(3) 0.0167(6) Uani 1 1 d . .
O6 O 0.0245(3) -0.1756(3) 0.1927(2) 0.0242(6) Uani 1 1 d . .
C6 C 0.2886(5) 0.0256(4) 1.0704(3) 0.0237(8) Uani 1 1 d . .
H6A H 0.3412 0.0378 1.1465 0.028 Uiso 1 1 d R U
O7 O -0.0877(4) -0.3597(3) 0.7526(3) 0.0274(6) Uani 1 1 d . .
C7 C 0.2212(5) 0.1208(4) 1.0377(3) 0.0253(8) Uani 1 1 d . .
H7A H 0.2195 0.2148 1.0878 0.030 Uiso 1 1 d R U
O8 O 0.3643(3) -0.1318(3) 0.6812(2) 0.0187(5) Uani 1 1 d . .
O9 O 0.0978(4) -0.3553(3) 0.2917(3) 0.0257(6) Uani 1 1 d . .
O10 O 0.3740(3) -0.1386(3) 0.2541(2) 0.0149(5) Uani 1 1 d . .
O11 O 0.3822(3) -0.1231(2) 0.4600(2) 0.0130(4) Uani 1 1 d . .
O12 O 0.2917(3) 0.0867(3) 0.6256(2) 0.0174(5) Uani 1 1 d . .
O13 O 0.1422(4) -0.4260(3) 0.5876(2) 0.0278(6) Uani 1 1 d . .
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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 O8 89.74(10) . .
O2 Ni1 N1 98.15(11) . .
O8 Ni1 N1 91.45(11) . .
O2 Ni1 O7 89.85(11) . .
O8 Ni1 O7 176.92(11) . .
N1 Ni1 O7 91.63(12) . .
O2 Ni1 O13 96.84(11) . .
O8 Ni1 O13 86.94(11) . .
N1 Ni1 O13 164.91(11) . .
O7 Ni1 O13 90.08(12) . .
O2 Ni1 O1 176.18(11) . .
O8 Ni1 O1 92.40(10) . .
N1 Ni1 O1 78.64(11) . .
O7 Ni1 O1 88.19(11) . .
O13 Ni1 O1 86.43(11) . .
C2 C1 C3 119.8(3) . 2_647
C2 C1 N3 116.6(3) . .
C3 C1 N3 123.5(3) 2_647 .
C4 O1 Ni1 114.3(2) . .
N2 N1 C5 105.9(3) . .
N2 N1 Ni1 140.2(2) . .
C5 N1 Ni1 113.8(2) . .
O12 Mo1 O8 105.00(12) . .
O12 Mo1 O11 99.98(11) . .
O8 Mo1 O11 102.80(11) . .
O12 Mo1 O10 98.76(11) . 2_656
O8 Mo1 O10 98.79(11) . 2_656
O11 Mo1 O10 146.51(10) . 2_656
O12 Mo1 O11 94.83(10) . 2_656
O8 Mo1 O11 159.90(10) . 2_656
O11 Mo1 O11 76.42(10) . 2_656
O10 Mo1 O11 74.55(9) 2_656 2_656
O12 Mo1 O4 164.61(10) . 1_655
O8 Mo1 O4 88.89(10) . 1_655
O11 Mo1 O4 82.96(9) . 1_655
O10 Mo1 O4 72.11(9) 2_656 1_655
O11 Mo1 O4 71.04(8) 2_656 1_655
O12 Mo1 Mo2 117.86(8) . 2_656
O8 Mo1 Mo2 117.36(8) . 2_656
O11 Mo1 Mo2 111.49(7) . 2_656
O10 Mo1 Mo2 35.06(7) 2_656 2_656
O11 Mo1 Mo2 47.60(6) 2_656 2_656
O4 Mo1 Mo2 47.98(6) 1_655 2_656
O12 Mo1 Mo1 99.14(8) . 2_656
O8 Mo1 Mo1 140.75(9) . 2_656
O11 Mo1 Mo1 41.90(7) . 2_656
O10 Mo1 Mo1 107.65(7) 2_656 2_656
O11 Mo1 Mo1 34.52(6) 2_656 2_656
O4 Mo1 Mo1 72.86(6) 1_655 2_656
Mo2 Mo1 Mo1 75.539(11) 2_656 2_656
O9 Mo2 O6 104.21(14) . .
O9 Mo2 O10 105.51(12) . .
O6 Mo2 O10 97.96(12) . .
O9 Mo2 O5 102.19(12) . .
O6 Mo2 O5 99.35(12) . .
O10 Mo2 O5 142.39(10) . .
O9 Mo2 O11 89.17(11) . .
O6 Mo2 O11 165.21(11) . .
O10 Mo2 O11 71.95(9) . .
O5 Mo2 O11 83.64(9) . .
O9 Mo2 O4 158.04(11) . 2_556
O6 Mo2 O4 97.60(11) . 2_556
O10 Mo2 O4 73.48(9) . 2_556
O5 Mo2 O4 71.32(9) . 2_556
O11 Mo2 O4 69.48(8) . 2_556
O9 Mo2 Mo1 117.99(9) . 2_656
O6 Mo2 Mo1 121.96(9) . 2_656
O10 Mo2 Mo1 35.72(7) . 2_656
O5 Mo2 Mo1 107.88(7) . 2_656
O11 Mo2 Mo1 44.07(6) . 2_656
O4 Mo2 Mo1 48.98(5) 2_556 2_656
C1 C2 C3 120.8(4) . .
N1 N2 C7 111.7(3) . .
Mo3 O2 Ni1 168.31(17) . .
O3 Mo3 O2 104.00(13) . .
O3 Mo3 O4 106.37(12) . .
O2 Mo3 O4 102.17(11) . .
O3 Mo3 O5 98.34(12) . .
O2 Mo3 O5 97.07(10) . .
O4 Mo3 O5 143.66(10) . .
O3 Mo3 O5 153.45(11) . 2_556
O2 Mo3 O5 101.06(11) . 2_556
O4 Mo3 O5 76.38(10) . 2_556
O5 Mo3 O5 69.81(10) . 2_556
O3 Mo3 O12 81.36(11) . 2_556
O2 Mo3 O12 171.00(10) . 2_556
O4 Mo3 O12 82.91(9) . 2_556
O5 Mo3 O12 74.82(9) . 2_556
O5 Mo3 O12 72.70(8) 2_556 2_556
C4 N3 C1 126.9(3) . .
C2 C3 C1 119.4(3) . 2_647
Mo3 O4 Mo2 103.44(10) . 2_556
Mo3 O4 Mo1 151.09(13) . 1_455
Mo2 O4 Mo1 83.04(8) 2_556 1_455
O1 C4 N3 124.0(3) . .
O1 C4 C5 118.0(3) . .
N3 C4 C5 117.9(3) . .
Mo2 O5 Mo3 144.14(13) . .
Mo2 O5 Mo3 105.61(10) . 2_556
Mo3 O5 Mo3 110.19(10) . 2_556
N1 C5 C6 111.0(3) . .
N1 C5 C4 114.2(3) . .
C6 C5 C4 134.7(3) . .
C7 C6 C5 103.9(3) . .
N2 C7 C6 107.4(3) . .
Mo1 O8 Ni1 142.20(14) . .
Mo2 O10 Mo1 109.22(11) . 2_656
Mo1 O11 Mo1 103.58(10) . 2_656
Mo1 O11 Mo2 135.82(11) . .
Mo1 O11 Mo2 88.33(8) 2_656 .
Mo1 O12 Mo3 130.64(13) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.044(2) .
Ni1 O8 2.051(2) .
Ni1 N1 2.056(3) .
Ni1 O7 2.061(3) .
Ni1 O13 2.065(3) .
Ni1 O1 2.071(2) .
C1 C2 1.382(5) .
C1 C3 1.383(5) 2_647
C1 N3 1.419(4) .
O1 C4 1.247(4) .
N1 N2 1.328(4) .
N1 C5 1.336(4) .
Mo1 O12 1.717(2) .
Mo1 O8 1.730(2) .
Mo1 O11 1.863(2) .
Mo1 O10 1.951(2) 2_656
Mo1 O11 2.196(2) 2_656
Mo1 O4 2.398(2) 1_655
Mo1 Mo2 3.1554(4) 2_656
Mo1 Mo1 3.1962(5) 2_656
Mo2 O9 1.702(3) .
Mo2 O6 1.706(2) .
Mo2 O10 1.920(2) .
Mo2 O5 1.923(2) .
Mo2 O11 2.331(2) .
Mo2 O4 2.362(2) 2_556
Mo2 Mo1 3.1554(4) 2_656
C2 C3 1.387(5) .
N2 C7 1.351(5) .
O2 Mo3 1.731(2) .
Mo3 O3 1.705(3) .
Mo3 O4 1.829(2) .
Mo3 O5 2.008(2) .
Mo3 O5 2.221(2) 2_556
Mo3 O12 2.441(2) 2_556
N3 C4 1.332(4) .
C3 C1 1.383(5) 2_647
O4 Mo2 2.362(2) 2_556
O4 Mo1 2.398(2) 1_455
C4 C5 1.474(5) .
O5 Mo3 2.221(2) 2_556
C5 C6 1.402(5) .
C6 C7 1.385(5) .
O10 Mo1 1.951(2) 2_656
O11 Mo1 2.196(2) 2_656
O12 Mo3 2.441(2) 2_556
