#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:23:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179325 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/22/4322274.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_4322274
loop_
_publ_author_name
'Pamela J. Hagrman'
'Jon Zubieta'
_publ_section_title
;
 Solid-State Coordination Chemistry of Metal Oxides: Hydrothermal
 Synthesis and Structural Characterization of o-Phenanthroline-Ligated
 Copper- and Zinc-Molybdenum Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4480
_journal_page_last               4485
_journal_paper_doi               10.1021/ic990340p
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H8 Mo N2 O4 Zn'
_chemical_formula_weight         405.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.702(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7714(7)
_cell_length_b                   6.4172(2)
_cell_length_c                   10.6524(10)
_cell_measurement_temperature    120(2)
_cell_volume                     589.17(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       'Bruker SMART-CCD'
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3907
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    3.114
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.286
_exptl_crystal_description       Block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_obs          0.0190
_refine_ls_shift/esd_max         -0.224
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0281P)²+0.2434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0485
_refine_ls_wR_factor_obs         0.0479
_reflns_number_observed          1412
_reflns_number_total             1520
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990340p_3.cif
_cod_data_source_block           MOXI-29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.2434P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.2434P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        589.17(7)
_cod_database_code               4322274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.49707(2) 0.2500 0.17387(2) 0.00629(8) Uani 1 d S .
Zn2 Zn 0.29617(3) 0.2500 -0.17236(3) 0.00782(9) Uani 1 d S .
O1 O 0.61441(15) 0.0231(2) 0.20968(13) 0.0147(3) Uani 1 d . .
O2 O 0.3554(3) 0.2500 0.2659(2) 0.0210(5) Uani 1 d S .
O3 O 0.4066(2) 0.2500 0.0123(2) 0.0173(4) Uani 1 d S .
N1 N 0.0738(3) 0.2500 -0.1239(2) 0.0101(4) Uani 1 d S .
N2 N 0.1487(2) 0.2500 -0.3578(2) 0.0088(4) Uani 1 d S .
C1 C 0.0398(3) 0.2500 -0.0073(3) 0.0118(5) Uani 1 d S .
C2 C -0.1136(3) 0.2500 0.0134(3) 0.0144(6) Uani 1 d S .
C3 C -0.2343(3) 0.2500 -0.0900(3) 0.0139(5) Uani 1 d S .
C4 C -0.2026(3) 0.2500 -0.2149(3) 0.0126(5) Uani 1 d S .
C5 C -0.0449(3) 0.2500 -0.2267(2) 0.0096(5) Uani 1 d S .
C6 C -0.3198(3) 0.2500 -0.3282(3) 0.0146(5) Uani 1 d S .
C7 C -0.2815(3) 0.2500 -0.4448(3) 0.0145(5) Uani 1 d S .
C8 C -0.1229(3) 0.2500 -0.4613(3) 0.0101(5) Uani 1 d S .
C9 C -0.0051(3) 0.2500 -0.3522(2) 0.0094(5) Uani 1 d S .
C10 C -0.0764(3) 0.2500 -0.5808(3) 0.0117(5) Uani 1 d S .
C11 C 0.0787(3) 0.2500 -0.5860(2) 0.0119(5) Uani 1 d S .
C12 C 0.1879(3) 0.2500 -0.4722(3) 0.0114(5) Uani 1 d S .
H12A H 0.2851(37) 0.2500 -0.4718(27) 0.000(7) Uiso 1 d S .
H1A H 0.1111(38) 0.2500 0.0501(32) 0.005(7) Uiso 1 d S .
H2A H -0.1310(42) 0.2500 0.1040(35) 0.019(9) Uiso 1 d S .
H11A H 0.1160(44) 0.2500 -0.6753(36) 0.022(10) Uiso 1 d S .
H3A H -0.3323(47) 0.2500 -0.0852(36) 0.023(10) Uiso 1 d S .
H6A H -0.4250(41) 0.2500 -0.3170(31) 0.012(8) Uiso 1 d S .
H10A H -0.1439(41) 0.2500 -0.6422(34) 0.011(8) Uiso 1 d S .
H7A H -0.3555(46) 0.2500 -0.5141(35) 0.021(9) Uiso 1 d S .
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'
Zn Zn 0.2839 1.4301 '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
O2 Mo1 O3 108.41(10) . . ?
O2 Mo1 O1 109.11(6) . 4_565 ?
O3 Mo1 O1 110.34(6) . 4_565 ?
O2 Mo1 O1 109.11(6) . . ?
O3 Mo1 O1 110.34(6) . . ?
O1 Mo1 O1 109.51(9) 4_565 . ?
O1 Zn2 O1 123.43(8) 3_655 2_655 ?
O1 Zn2 O3 93.38(5) 3_655 . ?
O1 Zn2 O3 93.38(5) 2_655 . ?
O1 Zn2 N1 117.76(4) 3_655 . ?
O1 Zn2 N1 117.76(4) 2_655 . ?
O3 Zn2 N1 93.40(9) . . ?
O1 Zn2 N2 90.49(5) 3_655 . ?
O1 Zn2 N2 90.49(5) 2_655 . ?
O3 Zn2 N2 171.82(8) . . ?
N1 Zn2 N2 78.41(9) . . ?
Mo1 O1 Zn2 155.46(8) . 3_655 ?
Mo1 O3 Zn2 178.34(13) . . ?
C1 N1 C5 118.7(2) . . ?
C1 N1 Zn2 127.3(2) . . ?
C5 N1 Zn2 114.0(2) . . ?
C12 N2 C9 118.0(2) . . ?
C12 N2 Zn2 129.0(2) . . ?
C9 N2 Zn2 113.0(2) . . ?
N1 C1 C2 122.3(2) . . ?
C3 C2 C1 119.4(3) . . ?
C2 C3 C4 119.8(2) . . ?
C3 C4 C5 116.9(2) . . ?
C3 C4 C6 124.0(2) . . ?
C5 C4 C6 119.1(3) . . ?
N1 C5 C4 122.9(2) . . ?
N1 C5 C9 117.6(2) . . ?
C4 C5 C9 119.5(2) . . ?
C7 C6 C4 121.0(3) . . ?
C6 C7 C8 121.8(2) . . ?
C9 C8 C10 117.2(2) . . ?
C9 C8 C7 118.7(2) . . ?
C10 C8 C7 124.2(2) . . ?
N2 C9 C8 123.1(2) . . ?
N2 C9 C5 116.9(2) . . ?
C8 C9 C5 120.0(2) . . ?
C11 C10 C8 119.5(2) . . ?
C10 C11 C12 119.3(2) . . ?
N2 C12 C11 122.9(2) . . ?
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 O2 1.720(2) . ?
Mo1 O3 1.756(2) . ?
Mo1 O1 1.7832(13) 4_565 ?
Mo1 O1 1.7832(13) . ?
Zn2 O1 1.9899(13) 3_655 ?
Zn2 O1 1.9899(13) 2_655 ?
Zn2 O3 2.025(2) . ?
Zn2 N1 2.108(2) . ?
Zn2 N2 2.151(2) . ?
O1 Zn2 1.9899(13) 3_655 ?
N1 C1 1.330(3) . ?
N1 C5 1.364(3) . ?
N2 C12 1.325(4) . ?
N2 C9 1.362(3) . ?
C1 C2 1.403(4) . ?
C2 C3 1.379(4) . ?
C3 C4 1.408(4) . ?
C4 C5 1.412(4) . ?
C4 C6 1.433(4) . ?
C5 C9 1.444(4) . ?
C6 C7 1.346(4) . ?
C7 C8 1.435(4) . ?
C8 C9 1.404(3) . ?
C8 C10 1.406(4) . ?
C10 C11 1.372(4) . ?
C11 C12 1.399(4) . ?
