#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319432.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_4319432
loop_
_publ_author_name
'Patrick C. McGowan'
'Thomas J. Podesta'
'Mark Thornton-Pett'
_publ_contact_author
;
   Patrick McGowan
   School of Chemistry 
   University of Leeds
   Leeds LS2 9JT
   UK
;
_publ_contact_author_email       patrickm@chem.leeds.ac.uk
_publ_contact_author_fax         '+44 (0)113 2336565'
_publ_contact_author_phone       '+44 (0)113 2336404'
_publ_section_title
;
 N-Monofunctionalized 1,4,7-Triazacyclononane Macrocycles as Building
 Blocks in Inorganic Crystal Engineering
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1445
_journal_page_last               1453
_journal_paper_doi               10.1021/ic0006854
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C9 H21 Mo N3 O4'
_chemical_formula_weight         331.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.52140(10)
_cell_length_b                   12.0922(3)
_cell_length_c                   14.3460(4)
_cell_measurement_reflns_used    31765
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      2.02
_cell_volume                     1304.77(5)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'KCCD (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '1 degree phi exposures'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2549
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.8386
_exptl_absorpt_correction_T_min  0.7118
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_coef       0.0127(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+0.5028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                2525
_reflns_number_total             31765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006854_2.cif
_cod_data_source_block           pm2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319432
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.00263(2) 0.273041(12) 0.619100(10) 0.01858(9) Uani 1 1 d . . .
O3 O -0.0211(2) 0.30729(12) 0.50094(10) 0.0241(3) Uani 1 1 d . . .
O1 O -0.1630(2) 0.34423(13) 0.67893(12) 0.0262(4) Uani 1 1 d . . .
O2 O 0.2047(2) 0.32919(13) 0.65424(12) 0.0245(3) Uani 1 1 d . . .
N1 N 0.0361(2) 0.15275(15) 0.75068(12) 0.0218(4) Uani 1 1 d . . .
N2 N -0.2069(2) 0.13336(16) 0.60403(13) 0.0226(4) Uani 1 1 d . . .
H2 H -0.3041 0.1642 0.5735 0.027 Uiso 1 1 calc R . .
N3 N 0.1475(2) 0.11670(15) 0.56826(13) 0.0222(4) Uani 1 1 d . . .
H3 H 0.2452 0.1411 0.5343 0.027 Uiso 1 1 calc R . .
C9 C -0.0244(4) 0.1853(2) 1.00048(17) 0.0416(6) Uani 1 1 d . . .
H9A H -0.1169 0.2388 0.9996 0.050 Uiso 1 1 calc R . .
H9B H -0.0001 0.1451 1.0559 0.050 Uiso 1 1 calc R . .
C4 C 0.0291(3) 0.06055(18) 0.50091(15) 0.0265(5) Uani 1 1 d . . .
H4A H 0.0843 -0.0095 0.4799 0.032 Uiso 1 1 calc R . .
H4B H 0.0110 0.1083 0.4456 0.032 Uiso 1 1 calc R . .
C7 C 0.0416(3) 0.22582(18) 0.83496(15) 0.0273(5) Uani 1 1 d . . .
H7A H -0.0711 0.2679 0.8380 0.033 Uiso 1 1 calc R . .
H7B H 0.1392 0.2799 0.8269 0.033 Uiso 1 1 calc R . .
C2 C -0.2688(3) 0.10210(19) 0.69856(16) 0.0247(5) Uani 1 1 d . . .
H2A H -0.3522 0.0390 0.6942 0.030 Uiso 1 1 calc R . .
H2B H -0.3325 0.1651 0.7273 0.030 Uiso 1 1 calc R . .
C5 C 0.2186(3) 0.04228(17) 0.64202(16) 0.0248(5) Uani 1 1 d . . .
H5A H 0.3431 0.0224 0.6271 0.030 Uiso 1 1 calc R . .
H5B H 0.1477 -0.0267 0.6437 0.030 Uiso 1 1 calc R . .
C1 C -0.1105(3) 0.07022(18) 0.75881(15) 0.0236(5) Uani 1 1 d . . .
H1A H -0.1487 0.0651 0.8247 0.028 Uiso 1 1 calc R . .
H1B H -0.0663 -0.0034 0.7395 0.028 Uiso 1 1 calc R . .
C3 C -0.1486(3) 0.03659(18) 0.54685(16) 0.0260(5) Uani 1 1 d . . .
H3A H -0.2388 0.0208 0.4984 0.031 Uiso 1 1 calc R . .
H3B H -0.1378 -0.0295 0.5872 0.031 Uiso 1 1 calc R . .
C6 C 0.2119(3) 0.09785(19) 0.73663(16) 0.0241(4) Uani 1 1 d . . .
H6A H 0.2310 0.0420 0.7861 0.029 Uiso 1 1 calc R . .
H6B H 0.3080 0.1535 0.7411 0.029 Uiso 1 1 calc R . .
C8 C 0.0679(3) 0.1673(2) 0.92667(17) 0.0335(5) Uani 1 1 d . . .
H8 H 0.1593 0.1132 0.9301 0.040 Uiso 1 1 calc R . .
O1S O 0.5026(3) 0.36088(14) 0.76640(11) 0.0298(3) Uani 1 1 d . . .
H2S H 0.433(4) 0.351(3) 0.726(2) 0.029(8) Uiso 1 1 d . . .
H1S H 0.583(4) 0.358(3) 0.738(2) 0.034(9) Uiso 1 1 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'
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
_geom_angle_publ_flag
O2 Mo1 O1 106.83(8) . . ?
O2 Mo1 O3 106.06(7) . . ?
O1 Mo1 O3 106.68(8) . . ?
O2 Mo1 N3 89.93(7) . . ?
O1 Mo1 N3 154.37(7) . . ?
O3 Mo1 N3 86.32(7) . . ?
O2 Mo1 N2 154.78(7) . . ?
O1 Mo1 N2 85.40(7) . . ?
O3 Mo1 N2 90.74(7) . . ?
N3 Mo1 N2 72.17(7) . . ?
O2 Mo1 N1 85.23(7) . . ?
O1 Mo1 N1 89.25(7) . . ?
O3 Mo1 N1 156.24(6) . . ?
N3 Mo1 N1 72.61(6) . . ?
N2 Mo1 N1 72.71(6) . . ?
C1 N1 C6 111.57(17) . . ?
C1 N1 C7 110.60(16) . . ?
C6 N1 C7 110.29(17) . . ?
C1 N1 Mo1 112.95(12) . . ?
C6 N1 Mo1 104.87(13) . . ?
C7 N1 Mo1 106.30(12) . . ?
C2 N2 C3 113.23(18) . . ?
C2 N2 Mo1 108.28(13) . . ?
C3 N2 Mo1 114.96(13) . . ?
C4 N3 C5 113.79(16) . . ?
C4 N3 Mo1 107.40(13) . . ?
C5 N3 Mo1 116.20(13) . . ?
N3 C4 C3 109.52(18) . . ?
N1 C7 C8 115.55(19) . . ?
N2 C2 C1 109.79(17) . . ?
N3 C5 C6 110.89(17) . . ?
N1 C1 C2 111.38(17) . . ?
N2 C3 C4 110.30(18) . . ?
N1 C6 C5 110.35(17) . . ?
C9 C8 C7 124.7(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 1.7392(15) . ?
Mo1 O1 1.7407(16) . ?
Mo1 O3 1.7541(14) . ?
Mo1 N3 2.3007(18) . ?
Mo1 N2 2.3201(18) . ?
Mo1 N1 2.3963(17) . ?
N1 C1 1.492(3) . ?
N1 C6 1.493(3) . ?
N1 C7 1.498(3) . ?
N2 C2 1.483(3) . ?
N2 C3 1.495(3) . ?
N3 C4 1.479(3) . ?
N3 C5 1.489(3) . ?
C9 C8 1.285(4) . ?
C4 C3 1.518(3) . ?
C7 C8 1.507(3) . ?
C2 C1 1.521(3) . ?
C5 C6 1.515(3) . ?
