#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/79/7027916.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027916
loop_
_publ_author_name
'Wong, Yee-Lok'
'Yan, Yan'
'Chan, Edith S. H.'
'Yang, Qingchuan'
'Mak, Thomas C. W.'
'Ng, Dennis K. P.'
_publ_section_title
;
 cis-Dioxo-tungsten(VI) and -molybdenum(VI) complexes with N2O2
 tetradentate ligands: synthesis, structure, electrochemistry and
 oxo-transfer properties
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3057
_journal_paper_doi               10.1039/a804425b
_journal_year                    1998
_chemical_formula_sum            'C20 H16 Mo N4 O8'
_chemical_formula_weight         536.31
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.172(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4745(4)
_cell_length_b                   11.4210(6)
_cell_length_c                   9.5782(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1030.43(8)
_computing_cell_refinement       'Biotex Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'Biotex Rigaku'
_computing_molecular_graphics    'Simens SHELXTL'
_computing_publication_material  'Simens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'IP Rigaku'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3343
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.188
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0000(23)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_obs          0.0551
_refine_ls_shift/esd_max         -1.681
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1211P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1575
_refine_ls_wR_factor_obs         0.1424
_reflns_number_observed          3267
_reflns_number_total             3343
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b804425sup1.cif
_cod_data_source_block           m1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1211P)^2^+0.0000P] 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^)+(0.1211P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7027916
loop_
_symmetry_equiv_pos_as_xyz
'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
Mo1 Mo 0.345747(10) 0.62377(2) 0.597765(10) 0.04396(4) Uani 1 d .
O1 O 0.52261(11) 0.62042(13) 0.57914(12) 0.0571(3) Uani 1 d .
O2 O 0.30976(15) 0.75535(11) 0.6700(2) 0.0569(3) Uani 1 d .
O3 O 0.35010(13) 0.52483(11) 0.76766(14) 0.0531(3) Uani 1 d .
O4 O 0.28319(11) 0.66548(11) 0.40174(12) 0.0521(3) Uani 1 d .
O5 O 0.0409(2) 0.0532(2) 0.8128(2) 0.1240(8) Uani 1 d .
O6 O -0.0265(2) 0.1434(3) 0.9935(2) 0.1380(8) Uani 1 d .
O7 O 0.6599(2) 0.5021(2) -0.0594(3) 0.0912(6) Uani 1 d .
O8 O 0.6182(2) 0.6818(2) -0.1178(2) 0.0807(5) Uani 1 d .
N1 N 0.31903(13) 0.43804(13) 0.4843(2) 0.0477(4) Uani 1 d .
N2 N 0.10971(12) 0.56851(13) 0.58776(15) 0.0458(3) Uani 1 d .
N3 N 0.0384(2) 0.1376(2) 0.8882(2) 0.0877(5) Uani 1 d .
N4 N 0.6014(2) 0.5957(2) -0.0455(2) 0.0704(5) Uani 1 d .
C1 C 0.3531(2) 0.6400(2) 0.2899(2) 0.0517(5) Uani 1 d .
C2 C 0.3525(2) 0.7259(2) 0.1841(2) 0.0597(6) Uani 1 d .
H2 H 0.2984(2) 0.7935(2) 0.1888(2) 0.072 Uiso 1 calc R
C3 C 0.4334(2) 0.7091(2) 0.0721(2) 0.0644(6) Uani 1 d .
H3 H 0.4365(2) 0.7660(2) 0.0031(2) 0.077 Uiso 1 calc R
C4 C 0.5083(2) 0.6062(2) 0.0665(2) 0.0564(4) Uani 1 d .
C5 C 0.5016(2) 0.5179(2) 0.1620(2) 0.0547(5) Uani 1 d .
H5 H 0.5496(2) 0.4480(2) 0.1514(2) 0.066 Uiso 1 calc R
C6 C 0.4220(2) 0.5329(2) 0.2762(2) 0.0511(5) Uani 1 d .
C7 C 0.4210(2) 0.4313(2) 0.3763(2) 0.0540(5) Uani 1 d .
H7A H 0.4004(2) 0.3607(2) 0.3216(2) 0.065 Uiso 1 calc R
H7B H 0.5159(2) 0.4229(2) 0.4246(2) 0.065 Uiso 1 calc R
C8 C 0.3577(2) 0.3385(2) 0.5840(2) 0.0545(5) Uani 1 d .
H8A H 0.3446(2) 0.2652(2) 0.5329(2) 0.065 Uiso 1 calc R
H8B H 0.4574(2) 0.3448(2) 0.6187(2) 0.065 Uiso 1 calc R
C9 C 0.2726(2) 0.3353(2) 0.7056(2) 0.0512(5) Uani 1 d .
C10 C 0.1946(2) 0.2368(2) 0.7375(2) 0.0606(6) Uani 1 d .
H10 H 0.1905(2) 0.1712(2) 0.6797(2) 0.073 Uiso 1 calc R
C11 C 0.1235(2) 0.2383(2) 0.8564(2) 0.0666(5) Uani 1 d .
C12 C 0.1273(2) 0.3327(2) 0.9450(2) 0.0657(6) Uani 1 d .
H12 H 0.0776(2) 0.3310(2) 1.0235(2) 0.079 Uiso 1 calc R
C13 C 0.2051(2) 0.4299(2) 0.9171(2) 0.0601(6) Uani 1 d .
H13 H 0.2099(2) 0.4939(2) 0.9775(2) 0.072 Uiso 1 calc R
C14 C 0.2771(2) 0.43164(15) 0.7970(2) 0.0462(4) Uani 1 d .
C15 C 0.1721(2) 0.4243(2) 0.4162(2) 0.0522(5) Uani 1 d .
H15A H 0.1519(2) 0.3418(2) 0.4003(2) 0.063 Uiso 1 calc R
H15B H 0.1633(2) 0.4633(2) 0.3257(2) 0.063 Uiso 1 calc R
C16 C 0.0664(2) 0.4749(2) 0.5049(2) 0.0513(5) Uani 1 d .
C17 C -0.0709(2) 0.4317(2) 0.5052(3) 0.0711(7) Uani 1 d .
H17 H -0.1016(2) 0.3677(2) 0.4500(3) 0.085 Uiso 1 calc R
C18 C -0.1613(2) 0.4866(4) 0.5903(2) 0.0726(10) Uani 1 d .
H18 H -0.2541(2) 0.4599(4) 0.5901(2) 0.087 Uiso 1 calc R
C19 C -0.1174(2) 0.5759(2) 0.6715(3) 0.0700(6) Uani 1 d .
H19 H -0.1779(2) 0.6101(2) 0.7300(3) 0.084 Uiso 1 calc R
C20 C 0.0202(2) 0.6185(2) 0.6686(2) 0.0568(4) Uani 1 d .
H20 H 0.0501(2) 0.6826(2) 0.7239(2) 0.068 Uiso 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'
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'
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
O1 Mo1 O2 107.70(7)
O1 Mo1 O4 95.99(5)
O2 Mo1 O4 96.96(6)
O1 Mo1 O3 98.02(6)
O2 Mo1 O3 99.04(6)
O4 Mo1 O3 154.39(5)
O1 Mo1 N2 160.98(6)
O2 Mo1 N2 91.30(6)
O4 Mo1 N2 80.55(5)
O3 Mo1 N2 79.22(5)
O1 Mo1 N1 89.41(6)
O2 Mo1 N1 162.46(6)
O4 Mo1 N1 76.94(5)
O3 Mo1 N1 81.86(5)
N2 Mo1 N1 71.58(5)
C14 O3 Mo1 132.27(11)
C1 O4 Mo1 125.59(10)
C15 N1 C7 109.71(14)
C15 N1 C8 110.66(14)
C7 N1 C8 105.61(13)
C15 N1 Mo1 110.09(11)
C7 N1 Mo1 108.50(10)
C8 N1 Mo1 112.14(11)
C20 N2 C16 120.03(15)
C20 N2 Mo1 122.00(12)
C16 N2 Mo1 117.71(10)
O5 N3 O6 125.0(3)
O5 N3 C11 117.4(2)
O6 N3 C11 117.6(2)
O7 N4 O8 123.7(2)
O7 N4 C4 117.9(2)
O8 N4 C4 118.3(2)
O4 C1 C6 122.5(2)
O4 C1 C2 117.1(2)
C6 C1 C2 120.4(2)
C3 C2 C1 119.7(2)
C4 C3 C2 118.4(2)
C5 C4 C3 122.8(2)
C5 C4 N4 120.3(2)
C3 C4 N4 116.9(2)
C4 C5 C6 119.9(2)
C1 C6 C5 118.4(2)
C1 C6 C7 125.4(2)
C5 C6 C7 116.3(2)
N1 C7 C6 116.79(15)
C9 C8 N1 113.6(2)
C10 C9 C14 118.4(2)
C10 C9 C8 122.3(2)
C14 C9 C8 119.1(2)
C11 C10 C9 119.0(2)
C12 C11 C10 122.5(2)
C12 C11 N3 118.1(2)
C10 C11 N3 119.5(2)
C11 C12 C13 119.6(2)
C12 C13 C14 119.3(2)
O3 C14 C13 120.1(2)
O3 C14 C9 118.8(2)
C13 C14 C9 121.1(2)
N1 C15 C16 111.33(15)
N2 C16 C17 119.9(2)
N2 C16 C15 116.98(14)
C17 C16 C15 123.2(2)
C18 C17 C16 118.4(2)
C19 C18 C17 121.1(2)
C18 C19 C20 119.5(2)
N2 C20 C19 121.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 O1 1.7046(11)
Mo1 O2 1.7042(13)
Mo1 O4 1.9658(11)
Mo1 O3 1.9779(13)
Mo1 N2 2.3157(12)
Mo1 N1 2.3842(15)
O3 C14 1.316(2)
O4 C1 1.351(2)
O5 N3 1.206(3)
O6 N3 1.238(3)
O7 N4 1.219(3)
O8 N4 1.223(3)
N1 C15 1.481(2)
N1 C7 1.492(2)
N1 C8 1.504(3)
N2 C20 1.337(2)
N2 C16 1.368(2)
N3 C11 1.455(3)
N4 C4 1.465(3)
C1 C6 1.399(3)
C1 C2 1.410(3)
C2 C3 1.396(3)
C3 C4 1.377(3)
C4 C5 1.368(3)
C5 C6 1.403(3)
C6 C7 1.506(3)
C8 C9 1.487(3)
C9 C10 1.398(3)
C9 C14 1.404(3)
C10 C11 1.384(3)
C11 C12 1.370(3)
C12 C13 1.375(3)
C13 C14 1.399(3)
C15 C16 1.497(3)
C16 C17 1.392(3)
C17 C18 1.393(4)
C18 C19 1.322(4)
C19 C20 1.394(3)
