#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/21/8102123.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_8102123
loop_
_publ_author_name
'Zhang, Qingwei'
'Schulzke, Carola'
'Schmidt, Hans-Georg'
'Noltemeyer, Mathias'
_publ_section_title
;
Crystal structure of dimethylformamide-diethanolateamine-dioxomolybdenum
(VI), MoO₂[O(CH₂)₂NH(CH₂)₂O][(CH₃)₂NCHO]
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              215
_journal_page_last               216
_journal_volume                  222
_journal_year                    2007
_chemical_formula_structural     MoO2[O(CH2)2NH(CH2)2O][(CH3)2NCHO]
_chemical_formula_sum            'C7 H16 Mo N2 O5'
_chemical_formula_weight         304.16
_chemical_name_systematic
; 
dimethylformamide-diethanolateamine-dioxomolybdenum(VI)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.6514(13)
_cell_length_b                   12.862(3)
_cell_length_c                   25.968(5)
_cell_measurement_temperature    103(2)
_cell_volume                     2210.1(8)
_computing_molecular_graphics    'Diamond [11]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997) [4]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [3]'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22638
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.7965
_exptl_absorpt_correction_T_min  0.7965
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0121P)²+7.2650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                2193
_reflns_number_total             2259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2006.cff
_cod_data_source_block           schu11
_cod_original_sg_symbol_H-M      C12/c1
_cod_database_code               8102123
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.02357(3) 0.367518(15) 0.148970(7) 0.00996(7) Uani 1 8 f d . . .
O2 O -0.0600(2) 0.22859(12) 0.16377(6) 0.0139(3) Uani 1 8 f d . . .
O3 O 0.1824(2) 0.34288(13) 0.10198(6) 0.0147(3) Uani 1 8 f d . . .
O4 O 0.1743(2) 0.39547(14) 0.20489(6) 0.0168(4) Uani 1 8 f d . . .
O1 O -0.0607(2) 0.50704(13) 0.13060(6) 0.0145(3) Uani 1 8 f d . . .
N1 N -0.2755(3) 0.38709(15) 0.18464(8) 0.0121(4) Uani 1 8 f d . . .
C3 C -0.3871(3) 0.28789(18) 0.18010(9) 0.0130(5) Uani 1 8 f d . . .
H3B H -0.4547 0.2786 0.1447 0.016 Uiso 1 8 f calc R . .
H3C H -0.4901 0.2851 0.2050 0.016 Uiso 1 8 f calc R . .
C4 C -0.2265(4) 0.20530(19) 0.19242(9) 0.0150(5) Uani 1 8 f d . . .
H4B H -0.1820 0.2051 0.2300 0.018 Uiso 1 8 f calc R . .
H4C H -0.2817 0.1358 0.1827 0.018 Uiso 1 8 f calc R . .
C1 C -0.2127(4) 0.55823(19) 0.15618(10) 0.0180(5) Uani 1 8 f d . . .
H1A H -0.2676 0.6180 0.1352 0.022 Uiso 1 8 f calc R . .
H1B H -0.1543 0.5846 0.1903 0.022 Uiso 1 8 f calc R . .
C2 C -0.3799(4) 0.48071(19) 0.16324(9) 0.0152(5) Uani 1 8 f d . . .
H2A H -0.4728 0.5082 0.1874 0.018 Uiso 1 8 f calc R . .
H2B H -0.4585 0.4652 0.1297 0.018 Uiso 1 8 f calc R . .
O5 O -0.2347(2) 0.34055(13) 0.07668(6) 0.0146(3) Uani 1 8 f d . . .
N2 N -0.3242(3) 0.37670(15) -0.00847(8) 0.0146(4) Uani 1 8 f d . . .
C5 C -0.1940(4) 0.36913(18) 0.03336(9) 0.0146(5) Uani 1 8 f d . . .
H5A H -0.0576 0.3872 0.0299 0.017 Uiso 1 8 f calc R . .
C7 C -0.5381(4) 0.3529(2) -0.00752(10) 0.0201(5) Uani 1 8 f d . . .
H7A H -0.5628 0.3300 0.0273 0.030 Uiso 1 8 f calc R . .
H7B H -0.5768 0.2974 -0.0324 0.030 Uiso 1 8 f calc R . .
H7C H -0.6186 0.4152 -0.0168 0.030 Uiso 1 8 f calc R . .
C6 C -0.2577(4) 0.4110(2) -0.05770(9) 0.0211(5) Uani 1 8 f d . . .
H6A H -0.1097 0.4112 -0.0552 0.032 Uiso 1 8 f calc R . .
H6B H -0.3085 0.4813 -0.0656 0.032 Uiso 1 8 f calc R . .
H6C H -0.3104 0.3634 -0.0853 0.032 Uiso 1 8 f calc R . .
H100 H -0.237(4) 0.398(2) 0.2154(11) 0.012(7) Uiso 1 8 f 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'
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
O4 Mo1 O3 106.87(8) . . ?
O4 Mo1 O2 100.45(8) . . ?
O3 Mo1 O2 100.44(7) . . ?
O4 Mo1 O1 98.32(8) . . ?
O3 Mo1 O1 100.38(7) . . ?
O2 Mo1 O1 146.43(7) . . ?
O4 Mo1 N1 95.24(8) . . ?
O3 Mo1 N1 157.89(8) . . ?
O2 Mo1 N1 74.97(7) . . ?
O1 Mo1 N1 75.81(7) . . ?
O4 Mo1 O5 170.62(7) . . ?
O3 Mo1 O5 82.15(7) . . ?
O2 Mo1 O5 79.99(6) . . ?
O1 Mo1 O5 77.12(6) . . ?
N1 Mo1 O5 75.77(7) . . ?
C4 O2 Mo1 123.71(14) . . ?
C1 O1 Mo1 121.16(14) . . ?
C2 N1 C3 117.62(18) . . ?
C2 N1 Mo1 109.46(14) . . ?
C3 N1 Mo1 108.85(14) . . ?
N1 C3 C4 104.54(18) . . ?
O2 C4 C3 108.06(18) . . ?
O1 C1 C2 108.39(19) . . ?
N1 C2 C1 105.05(19) . . ?
C5 O5 Mo1 117.07(15) . . ?
C5 N2 C7 122.0(2) . . ?
C5 N2 C6 120.6(2) . . ?
C7 N2 C6 117.4(2) . . ?
O5 C5 N2 125.6(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 O4 1.7168(17) . ?
Mo1 O3 1.7225(17) . ?
Mo1 O2 1.9217(17) . ?
Mo1 O1 1.9256(17) . ?
Mo1 N1 2.292(2) . ?
Mo1 O5 2.4376(18) . ?
O2 C4 1.427(3) . ?
O1 C1 1.425(3) . ?
N1 C2 1.471(3) . ?
N1 C3 1.475(3) . ?
C3 C4 1.517(3) . ?
C1 C2 1.519(3) . ?
O5 C5 1.239(3) . ?
N2 C5 1.322(3) . ?
N2 C7 1.458(3) . ?
N2 C6 1.462(3) . ?
