#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/20/8102003.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_8102003
loop_
_publ_author_name
'Peng, Z.-S.'
'Jiang, W.-J.'
'Deng, Q.'
'Long, Y.-F.'
'Cai, T.-J.'
_publ_section_title
;
Refinement of the crystal structure of catena-[(1,10-phenanthroline-
N,N')-(μ³-molybdato(VI))copper(II)] monohydrate, Cu(C₂H₁₀N₂)
(MoO₄) · H₂O
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              335
_journal_page_last               336
_journal_volume                  221
_journal_year                    2006
_chemical_formula_moiety         'C12 H8 Cu Mo N2 O4, H2 O'
_chemical_formula_structural     'Cu(C~12~H~10~N~2~)(MoO~4~) &#x00B7; H~2~O'
_chemical_formula_sum            'C12 H10 Cu Mo N2 O5'
_chemical_formula_weight         421.70
_chemical_name_systematic
; 
catena-[(1,10-phenanthroline)(μ₃-molybdato(VI))copper(II)] monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.271(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.147(3)
_cell_length_b                   5.8897(11)
_cell_length_c                   16.221(3)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     1315.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.87
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD II'
_diffrn_measurement_method       omega
_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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11008
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.592
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0228
_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)+(0.0285P)²+0.8410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                2860
_reflns_number_total             3304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1817.cff
_cod_data_source_block           '[Cu(MoO4)(C12H10N2)]H2O'
_cod_original_sg_symbol_H-M      P12(1)/n1
_cod_original_formula_sum        'C12 H10 Cu1 Mo1 N2 O5'
_cod_database_code               8102003
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.872034(13) 0.22461(3) 0.015275(12) 0.02307(7) Uani 1 4 e d . . .
O1 O 0.85180(11) 0.4868(3) 0.05976(10) 0.0302(3) Uani 1 4 e d . . .
O2 O 0.96578(13) 0.2517(3) -0.03918(12) 0.0366(4) Uani 1 4 e d . . .
O3 O 0.76572(13) 0.1475(3) -0.05488(12) 0.0446(4) Uani 1 4 e d . . .
O4 O 0.90085(12) 0.0179(3) 0.09646(11) 0.0355(4) Uani 1 4 e d . . .
Cu1 Cu 0.966540(19) 0.73343(4) 0.127915(17) 0.02390(8) Uani 1 4 e d . . .
N1 N 1.04754(13) 0.4678(3) 0.18639(11) 0.0269(4) Uani 1 4 e d . . .
N2 N 0.91774(14) 0.7289(3) 0.23466(12) 0.0266(4) Uani 1 4 e d . . .
C1 C 1.11103(17) 0.3369(4) 0.16005(15) 0.0323(5) Uani 1 4 e d . . .
H1A H 1.1270 0.3714 0.1090 0.039 Uiso 1 4 e calc R . .
C2 C 1.15479(18) 0.1492(5) 0.20608(16) 0.0366(6) Uani 1 4 e d . . .
H2A H 1.1987 0.0607 0.1854 0.044 Uiso 1 4 e calc R . .
C3 C 1.13302(17) 0.0961(4) 0.28126(16) 0.0365(6) Uani 1 4 e d . . .
H3A H 1.1627 -0.0270 0.3128 0.044 Uiso 1 4 e calc R . .
C4 C 1.06507(17) 0.2296(4) 0.31086(15) 0.0305(5) Uani 1 4 e d . . .
C5 C 1.03508(19) 0.1863(5) 0.38774(16) 0.0375(6) Uani 1 4 e d . . .
H5A H 1.0621 0.0651 0.4218 0.045 Uiso 1 4 e calc R . .
C6 C 0.96786(18) 0.3193(5) 0.41179(15) 0.0364(6) Uani 1 4 e d . . .
H6A H 0.9488 0.2858 0.4616 0.044 Uiso 1 4 e calc R . .
C7 C 0.92589(16) 0.5093(4) 0.36226(14) 0.0289(5) Uani 1 4 e d . . .
C8 C 0.85638(17) 0.6570(5) 0.38307(15) 0.0355(5) Uani 1 4 e d . . .
H8A H 0.8351 0.6345 0.4326 0.043 Uiso 1 4 e calc R . .
C9 C 0.82049(18) 0.8324(5) 0.33056(16) 0.0365(5) Uani 1 4 e d . . .
H9A H 0.7745 0.9299 0.3439 0.044 Uiso 1 4 e calc R . .
C10 C 0.85332(17) 0.8649(4) 0.25634(15) 0.0326(5) Uani 1 4 e d . . .
H10A H 0.8290 0.9862 0.2212 0.039 Uiso 1 4 e calc R . .
C11 C 1.02469(15) 0.4130(4) 0.26085(13) 0.0253(4) Uani 1 4 e d . . .
C12 C 0.95405(15) 0.5546(4) 0.28655(13) 0.0247(4) Uani 1 4 e d . . .
O1W O 0.68606(16) -0.2763(3) -0.04179(16) 0.0555(6) Uani 1 4 e d . . .
H2 H 0.7081 -0.1361 -0.0491 0.075 Uiso 1 4 e d . . .
H1 H 0.7330 -0.3562 -0.0073 0.075 Uiso 1 4 e 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'
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'
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
_geom_angle_publ_flag
O3 Mo1 O1 107.63(8) . . ?
O3 Mo1 O2 109.62(9) . . ?
O1 Mo1 O2 109.81(7) . . ?
O3 Mo1 O4 109.05(9) . . ?
O1 Mo1 O4 109.30(8) . . ?
O2 Mo1 O4 111.35(8) . . ?
Mo1 O1 Cu1 126.71(8) . . ?
Mo1 O2 Cu1 161.80(13) . 3_765 ?
Mo1 O4 Cu1 144.03(9) . 1_545 ?
O2 Cu1 O4 93.18(7) 3_765 1_565 ?
O2 Cu1 N2 170.08(8) 3_765 . ?
O4 Cu1 N2 89.98(7) 1_565 . ?
O2 Cu1 N1 93.47(7) 3_765 . ?
O4 Cu1 N1 167.21(8) 1_565 . ?
N2 Cu1 N1 81.73(7) . . ?
O2 Cu1 O1 95.09(7) 3_765 . ?
O4 Cu1 O1 100.37(7) 1_565 . ?
N2 Cu1 O1 93.59(7) . . ?
N1 Cu1 O1 89.91(7) . . ?
C1 N1 C11 117.69(19) . . ?
C1 N1 Cu1 130.21(16) . . ?
C11 N1 Cu1 111.89(14) . . ?
C10 N2 C12 118.8(2) . . ?
C10 N2 Cu1 128.11(16) . . ?
C12 N2 Cu1 113.01(14) . . ?
N1 C1 C2 122.5(2) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.8(2) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.3(2) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C11 C4 C3 117.1(2) . . ?
C11 C4 C5 118.8(2) . . ?
C3 C4 C5 124.1(2) . . ?
C6 C5 C4 121.1(2) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 119.5 . . ?
C5 C6 C7 121.3(2) . . ?
C5 C6 H6A 119.3 . . ?
C7 C6 H6A 119.3 . . ?
C12 C7 C8 116.5(2) . . ?
C12 C7 C6 118.6(2) . . ?
C8 C7 C6 124.9(2) . . ?
C9 C8 C7 119.9(2) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 119.5(2) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
N2 C10 C9 122.1(2) . . ?
N2 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
N1 C11 C4 123.6(2) . . ?
N1 C11 C12 116.33(19) . . ?
C4 C11 C12 120.1(2) . . ?
N2 C12 C7 123.2(2) . . ?
N2 C12 C11 116.79(19) . . ?
C7 C12 C11 120.1(2) . . ?
H2 O1W H1 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O3 1.7256(18) . ?
Mo1 O1 1.7557(16) . ?
Mo1 O2 1.7615(16) . ?
Mo1 O4 1.7711(16) . ?
O1 Cu1 2.2677(16) . ?
O2 Cu1 1.9049(16) 3_765 ?
O4 Cu1 1.9269(16) 1_545 ?
Cu1 O2 1.9049(16) 3_765 ?
Cu1 O4 1.9269(16) 1_565 ?
Cu1 N2 2.0061(19) . ?
Cu1 N1 2.0398(19) . ?
N1 C1 1.327(3) . ?
N1 C11 1.359(3) . ?
N2 C10 1.320(3) . ?
N2 C12 1.352(3) . ?
C1 C2 1.397(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.361(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.409(3) . ?
C3 H3A 0.9300 . ?
C4 C11 1.392(3) . ?
C4 C5 1.429(3) . ?
C5 C6 1.356(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.425(3) . ?
C6 H6A 0.9300 . ?
C7 C12 1.401(3) . ?
C7 C8 1.411(3) . ?
C8 C9 1.361(4) . ?
C8 H8A 0.9300 . ?
C9 C10 1.400(3) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.435(3) . ?
O1W H2 0.9006 . ?
O1W H1 0.8968 . ?
