#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:08:47 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193797 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/16/7041619.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_7041619
loop_
_publ_author_name
'Wang, Xiu-Li'
'Zhang, Rui'
'Wang, Xiang'
'Lin, Hong-Yan'
'Liu, Guo-Cheng'
'Zhang, Hui-Xiu'
_publ_section_title
;
 Three novel and various isopolymolybdate-based hybrids built from the
 carboxyl oxygen atoms of in situ ligands: substituent-tuned assembly,
 architectures and properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1965
_journal_page_last               1974
_journal_paper_doi               10.1039/c6dt04185j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C11 H7 Cu Mo2 N6 O8'
_chemical_formula_sum            'C11 H7 Cu Mo2 N6 O8'
_chemical_formula_weight         606.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1931(16)
_cell_length_b                   11.4242(7)
_cell_length_c                   7.3164(4)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.321
_cell_measurement_theta_min      3.364
_cell_volume                     1670.51(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4662
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.038
_exptl_absorpt_coefficient_mu    2.799
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0243
_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)+(0.0362P)²+2.8987P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1421
_reflns_number_total             1479
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04185j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7041618--7041620.cif.'
_cod_database_code               7041619
_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_max   0.679
_shelx_estimated_absorpt_t_min   0.618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C7(H7)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_refinement_flags_occupancy
Mo1 Mo 0.57191(2) -1.02057(2) 0.40438(3) 0.01332(12) Uani 1 1 d . . .
Cu1 Cu 0.2500 -0.2500 0.5000 0.0460(2) Uani 1 2 d S T P
O1 O 0.65223(11) -0.9747(2) 0.4283(3) 0.0293(5) Uani 1 1 d . . .
O2 O 0.54322(10) -0.97396(15) 0.6386(3) 0.0172(4) Uani 1 1 d . . .
O3 O 0.57917(11) -1.16688(19) 0.4425(3) 0.0274(5) Uani 1 1 d . . .
O4 O 0.54768(9) -0.82889(16) 0.3502(2) 0.0181(4) Uani 1 1 d . . .
N1 N 0.29638(13) -0.3113(2) 0.3186(4) 0.0323(6) Uani 1 1 d . . .
N2 N 0.37830(11) -0.4085(2) 0.2344(3) 0.0217(5) Uani 1 1 d . . .
N3 N 0.32197(15) -0.4571(3) 0.1367(5) 0.0400(7) Uani 1 1 d . . .
C1 C 0.5000 -0.4036(3) 0.2500 0.0202(8) Uani 1 2 d S T P
H1 H 0.5000 -0.3222 0.2500 0.024 Uiso 1 2 calc RS T P
C2 C 0.44075(14) -0.4671(2) 0.2393(4) 0.0188(6) Uani 1 1 d . . .
C3 C 0.44006(14) -0.5881(2) 0.2409(4) 0.0193(6) Uani 1 1 d . . .
H3 H 0.3999 -0.6285 0.2360 0.023 Uiso 1 1 calc R . .
C4 C 0.5000 -0.7795(3) 0.2500 0.0160(8) Uani 1 2 d S T P
C5 C 0.5000 -0.6483(3) 0.2500 0.0180(8) Uani 1 2 d S T P
C6 C 0.36194(14) -0.3222(2) 0.3403(4) 0.0222(6) Uani 1 1 d . . .
H6 H 0.3920 -0.2765 0.4177 0.027 Uiso 1 1 calc R . .
C7 C 0.27436(17) -0.3952(3) 0.1921(6) 0.0431(9) Uani 1 1 d . . .
H7 H 0.2293 -0.4073 0.1490 0.052 Uiso 1 1 calc R . .
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
O1 Mo1 O2 163.42(9) . 5_636
O1 Mo1 O2 104.90(10) . 6_535
O1 Mo1 O2 102.98(10) . .
O1 Mo1 O3 103.25(11) . .
O1 Mo1 O4 84.18(9) . .
O2 Mo1 O2 73.01(9) . 5_636
O2 Mo1 O2 142.98(11) 6_535 .
O2 Mo1 O2 73.29(8) 6_535 5_636
O2 Mo1 O4 80.23(7) 6_535 .
O2 Mo1 O4 78.87(7) . .
O3 Mo1 O2 98.81(8) . .
O3 Mo1 O2 93.30(8) . 5_636
O3 Mo1 O2 97.99(9) . 6_535
O3 Mo1 O4 172.56(9) . .
O4 Mo1 O2 79.27(6) . 5_636
N1 Cu1 N1 180.0 . 7_546
Mo1 O2 Mo1 106.99(9) . 5_636
Mo1 O2 Mo1 141.35(11) 6_536 .
Mo1 O2 Mo1 106.60(8) 6_536 5_636
C4 O4 Mo1 131.60(19) . .
C6 N1 Cu1 123.2(2) . .
C6 N1 C7 103.9(2) . .
C7 N1 Cu1 126.8(2) . .
N3 N2 C2 119.2(2) . .
C6 N2 N3 110.4(2) . .
C6 N2 C2 129.0(2) . .
C7 N3 N2 102.2(3) . .
C2 C1 C2 117.2(4) . 2_655
C1 C2 N2 120.5(3) . .
C3 C2 N2 117.4(2) . .
C3 C2 C1 122.0(3) . .
C2 C3 C5 119.1(3) . .
O4 C4 O4 126.7(3) . 2_655
O4 C4 C5 116.67(17) . .
O4 C4 C5 116.67(17) 2_655 .
C3 C5 C3 120.5(4) 2_655 .
C3 C5 C4 119.77(18) 2_655 .
C3 C5 C4 119.77(18) . .
N1 C6 N2 109.3(3) . .
N3 C7 N1 114.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.690(2) .
Mo1 O2 2.302(2) 5_636
Mo1 O2 1.9592(19) .
Mo1 O2 1.949(2) 6_535
Mo1 O3 1.698(2) .
Mo1 O4 2.2664(18) .
Cu1 N1 1.867(3) .
Cu1 N1 1.867(3) 7_546
O2 Mo1 2.302(2) 5_636
O2 Mo1 1.949(2) 6_536
O4 C4 1.257(2) .
N1 C6 1.316(4) .
N1 C7 1.362(4) .
N2 N3 1.372(4) .
N2 C2 1.424(4) .
N2 C6 1.325(4) .
N3 C7 1.304(5) .
C1 C2 1.392(4) .
C1 C2 1.392(4) 2_655
C2 C3 1.382(4) .
C3 C5 1.386(3) .
C4 O4 1.257(2) 2_655
C4 C5 1.499(5) .
C5 C3 1.386(3) 2_655
