#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:25:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180038 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/32/7033217.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_7033217
loop_
_publ_author_name
'Sengupta, Dolan'
'Gangopadhyay, Snigdha'
'Drew, Michael G. B.'
'Gangopadhyay, Pijush Kanti'
_publ_section_title
;
 Thiohydrazide complexes of molybdenum and their relevance to reduction of
 dinitrogen to ammonia.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1323
_journal_page_last               1331
_journal_paper_doi               10.1039/c4dt01945h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C18 H20 Mo2 N2 O9 S3'
_chemical_formula_weight         696.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.497(7)
_cell_angle_beta                 87.429(5)
_cell_angle_gamma                71.028(6)
_cell_formula_units_Z            1
_cell_length_a                   7.2719(4)
_cell_length_b                   8.8902(7)
_cell_length_c                   10.5788(7)
_cell_measurement_reflns_used    4273
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.61
_cell_volume                     599.59(8)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0204
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4273
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.957
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.762
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.762
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0587P)²+1.7427P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                3008
_reflns_number_total             3361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01945h2.cif
_cod_data_source_block           IIc
_cod_depositor_comments
'Adding full bibliography for 7033215--7033217.cif.'
_cod_original_cell_volume        599.59(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7033217
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O11 O 1.0351(3) -0.2293(2) 0.33986(19) 0.0225(4) Uani 1 1 d .
C12 C 1.1915(4) -0.3531(3) 0.3232(3) 0.0238(5) Uani 1 1 d .
C13 C 1.2805(4) -0.3273(4) 0.1991(3) 0.0275(6) Uani 1 1 d .
C14 C 1.4529(5) -0.4602(6) 0.1961(5) 0.0518(12) Uani 1 1 d .
H14 H 1.5163 -0.4460 0.1163 0.062 Uiso 1 1 calc R
C15 C 1.5282(5) -0.6094(5) 0.3082(7) 0.0660(17) Uani 1 1 d .
H15 H 1.6401 -0.6952 0.3039 0.079 Uiso 1 1 calc R
C16 C 1.4353(6) -0.6298(4) 0.4271(6) 0.0607(15) Uani 1 1 d .
H16 H 1.4862 -0.7305 0.5027 0.073 Uiso 1 1 calc R
C17 C 1.2687(5) -0.5046(4) 0.4367(4) 0.0370(8) Uani 1 1 d .
H17 H 1.2087 -0.5209 0.5179 0.044 Uiso 1 1 calc R
C18 C 1.2075(4) -0.1718(4) 0.0765(3) 0.0270(6) Uani 1 1 d .
S19 S 1.3957(2) -0.1555(2) -0.02902(14) 0.0230(3) Uani 0.50 1 d P
O19 O 1.3035(7) -0.1130(5) -0.0308(4) 0.0211(8) Uani 0.50 1 d P
N20 N 1.0240(4) -0.0722(3) 0.0608(2) 0.0240(5) Uani 1 1 d .
C23 C 1.1444(8) 0.2999(6) 0.1412(4) 0.0587(12) Uani 1 1 d .
H23A H 1.1112 0.3231 0.0476 0.088 Uiso 1 1 calc R
H23B H 1.2739 0.3023 0.1510 0.088 Uiso 1 1 calc R
H23C H 1.0535 0.3854 0.1691 0.088 Uiso 1 1 calc R
C24 C 1.1814(4) 0.0960(4) 0.4079(3) 0.0276(6) Uani 1 1 d .
H24A H 1.0847 0.1923 0.4196 0.041 Uiso 1 1 calc R
H24B H 1.3085 0.1048 0.4142 0.041 Uiso 1 1 calc R
H24C H 1.1763 -0.0081 0.4777 0.041 Uiso 1 1 calc R
O1 O 0.7589(3) -0.2492(3) 0.1845(2) 0.0319(5) Uani 1 1 d .
O3 O 0.6220(3) -0.0245(3) 0.3135(2) 0.0336(5) Uani 1 1 d .
O21 O 0.9171(3) 0.1159(3) 0.2347(2) 0.0285(4) Uani 1 1 d .
Mo1 Mo 0.80229(3) -0.08879(3) 0.21594(2) 0.01961(8) Uani 1 1 d .
S22 S 1.13443(10) 0.09387(9) 0.24512(7) 0.02380(14) Uani 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
C12 O11 Mo1 127.50(17) . .
O11 C12 C17 117.2(3) . .
O11 C12 C13 121.8(3) . .
C17 C12 C13 120.9(3) . .
C12 C13 C14 117.2(3) . .
C12 C13 C18 123.7(2) . .
C14 C13 C18 119.2(3) . .
C15 C14 C13 121.7(4) . .
C14 C15 C16 119.2(3) . .
C15 C16 C17 121.8(4) . .
C16 C17 C12 119.3(4) . .
N20 C18 O19 111.4(3) . .
N20 C18 C13 120.3(2) . .
O19 C18 C13 128.3(3) . .
N20 C18 S19 130.8(3) . .
O19 C18 S19 19.38(19) . .
C13 C18 S19 108.9(2) . .
O19 S19 C18 42.8(4) . .
O19 S19 Mo1 52.9(4) . 2_755
C18 S19 Mo1 95.60(13) . 2_755
S19 O19 C18 117.8(5) . .
S19 O19 Mo1 112.6(5) . 2_755
C18 O19 Mo1 129.4(3) . 2_755
C18 N20 N20 113.7(3) . 2_755
C18 N20 Mo1 127.48(19) . .
N20 N20 Mo1 118.1(2) 2_755 .
S22 O21 Mo1 123.39(11) . .
O1 Mo1 O3 105.90(11) . .
O1 Mo1 O11 97.35(10) . .
O3 Mo1 O11 106.26(9) . .
O1 Mo1 O19 100.58(14) . 2_755
O3 Mo1 O19 98.85(15) . 2_755
O11 Mo1 O19 143.66(14) . 2_755
O1 Mo1 N20 91.47(9) . .
O3 Mo1 N20 159.33(11) . .
O11 Mo1 N20 81.93(8) . .
O19 Mo1 N20 66.33(14) 2_755 .
O1 Mo1 O21 168.23(9) . .
O3 Mo1 O21 85.86(10) . .
O11 Mo1 O21 78.26(8) . .
O19 Mo1 O21 77.81(13) 2_755 .
N20 Mo1 O21 77.15(8) . .
O1 Mo1 S19 100.17(9) . 2_755
O3 Mo1 S19 85.09(9) . 2_755
O11 Mo1 S19 155.61(7) . 2_755
O19 Mo1 S19 14.49(11) 2_755 2_755
N20 Mo1 S19 80.80(7) . 2_755
O21 Mo1 S19 81.20(6) . 2_755
O21 S22 C24 105.20(13) . .
O21 S22 C23 103.70(19) . .
C24 S22 C23 98.95(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O11 C12 1.359(3) .
O11 Mo1 1.9415(19) .
C12 C17 1.398(4) .
C12 C13 1.412(4) .
C13 C14 1.425(4) .
C13 C18 1.465(5) .
C14 C15 1.378(7) .
C15 C16 1.381(8) .
C16 C17 1.383(5) .
C18 N20 1.318(4) .
C18 O19 1.334(5) .
C18 S19 1.736(3) .
S19 O19 0.651(4) .
S19 Mo1 2.4028(16) 2_755
O19 Mo1 2.076(4) 2_755
N20 N20 1.400(5) 2_755
N20 Mo1 2.248(2) .
C23 S22 1.781(4) .
C24 S22 1.778(3) .
O1 Mo1 1.701(2) .
O3 Mo1 1.713(2) .
O21 S22 1.532(2) .
O21 Mo1 2.306(2) .
Mo1 O19 2.076(4) 2_755
Mo1 S19 2.4027(16) 2_755
