#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:25:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180038 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/32/7033215.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_7033215
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            'C39 H36 Mo N6 O3 S3'
_chemical_formula_weight         828.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.6005(5)
_cell_length_b                   13.6005(5)
_cell_length_c                   11.9425(3)
_cell_measurement_reflns_used    13548
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.43
_cell_volume                     1913.09(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0794
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13548
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.43
_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    0.552
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.566
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0423
_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)+(0.0365P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                3026
_reflns_number_total             3725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01945h2.cif
_cod_data_source_block           IIa
_cod_depositor_comments
'Adding full bibliography for 7033215--7033217.cif.'
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7033215
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
Mo1 Mo 0.6667 0.3333 0.77828(2) 0.01442(10) Uani 1 3 d S
S20 S 0.82507(5) 0.43976(5) 0.65313(4) 0.01804(13) Uani 1 1 d .
N12 N 0.90642(16) 0.48571(16) 0.85874(13) 0.0181(4) Uani 1 1 d .
O150 O 1.11176(15) 0.63622(16) 0.91241(12) 0.0278(4) Uani 1 1 d D
H150 H 1.0443(16) 0.583(2) 0.918(2) 0.039(9) Uiso 1 1 d D
N11 N 0.80151(15) 0.39911(16) 0.87925(13) 0.0174(4) Uani 1 1 d .
H11 H 0.7912 0.3681 0.9442 0.021 Uiso 1 1 calc R
C13 C 0.92702(18) 0.51709(19) 0.75199(15) 0.0158(4) Uani 1 1 d .
C14 C 1.04009(19) 0.61060(19) 0.72174(16) 0.0172(4) Uani 1 1 d .
C15 C 1.12713(19) 0.6655(2) 0.80204(16) 0.0205(5) Uani 1 1 d .
C16 C 1.2341(2) 0.7510(2) 0.77011(18) 0.0271(5) Uani 1 1 d .
H16 H 1.2907 0.7865 0.8238 0.033 Uiso 1 1 calc R
C19 C 1.0660(2) 0.6470(2) 0.60998(17) 0.0218(5) Uani 1 1 d .
H19 H 1.0098 0.6129 0.5557 0.026 Uiso 1 1 calc R
C17 C 1.2574(2) 0.7839(2) 0.65937(19) 0.0299(6) Uani 1 1 d .
H17 H 1.3297 0.8407 0.6387 0.036 Uiso 1 1 calc R
C18 C 1.1728(2) 0.7320(2) 0.57875(18) 0.0261(5) Uani 1 1 d .
H18 H 1.1881 0.7545 0.5043 0.031 Uiso 1 1 calc R
C25 C 0.8486(3) 0.0781(4) 0.8736(3) 0.0707(12) Uani 1 1 d .
H25 H 0.8253 0.0493 0.9454 0.085 Uiso 1 1 calc R
C23 C 0.8722(4) 0.0484(5) 0.6872(4) 0.0846(16) Uani 1 1 d .
H23 H 0.8656 -0.0008 0.6299 0.101 Uiso 1 1 calc R
C26 C 0.8917(4) 0.1926(4) 0.8537(4) 0.0725(13) Uani 1 1 d .
H26 H 0.8977 0.2414 0.9113 0.087 Uiso 1 1 calc R
C22 C 0.9136(4) 0.1576(6) 0.6642(4) 0.0931(18) Uani 1 1 d .
H22 H 0.9348 0.1835 0.5913 0.112 Uiso 1 1 calc R
C24 C 0.8400(3) 0.0080(3) 0.7896(4) 0.0717(12) Uani 1 1 d .
H24 H 0.8115 -0.0688 0.8037 0.086 Uiso 1 1 calc R
C21 C 0.9254(3) 0.2325(4) 0.7468(5) 0.0798(14) Uani 1 1 d .
H21 H 0.9559 0.3092 0.7307 0.096 Uiso 1 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'
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 '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'
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
N11 Mo1 N11 87.23(7) 3_665 .
N11 Mo1 N11 87.22(7) 3_665 2_655
N11 Mo1 N11 87.23(7) . 2_655
N11 Mo1 S20 142.46(5) 3_665 .
N11 Mo1 S20 76.18(5) . .
N11 Mo1 S20 124.52(6) 2_655 .
N11 Mo1 S20 124.52(6) 3_665 2_655
N11 Mo1 S20 142.46(5) . 2_655
N11 Mo1 S20 76.18(5) 2_655 2_655
S20 Mo1 S20 85.836(19) . 2_655
N11 Mo1 S20 76.18(5) 3_665 3_665
N11 Mo1 S20 124.52(6) . 3_665
N11 Mo1 S20 142.46(6) 2_655 3_665
S20 Mo1 S20 85.836(19) . 3_665
S20 Mo1 S20 85.835(19) 2_655 3_665
C13 S20 Mo1 98.40(7) . .
C13 N12 N11 114.69(17) . .
C15 O150 H150 105.4(18) . .
N12 N11 Mo1 128.22(12) . .
N12 N11 H11 115.9 . .
Mo1 N11 H11 115.9 . .
N12 C13 C14 118.38(18) . .
N12 C13 S20 119.05(17) . .
C14 C13 S20 122.35(14) . .
C19 C14 C15 117.5(2) . .
C19 C14 C13 120.53(19) . .
C15 C14 C13 121.91(18) . .
O150 C15 C16 117.0(2) . .
O150 C15 C14 122.5(2) . .
C16 C15 C14 120.48(19) . .
C17 C16 C15 120.6(2) . .
C17 C16 H16 119.7 . .
C15 C16 H16 119.7 . .
C18 C19 C14 121.7(2) . .
C18 C19 H19 119.2 . .
C14 C19 H19 119.2 . .
C16 C17 C18 120.0(2) . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C19 C18 C17 119.7(2) . .
C19 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C24 C25 C26 120.5(4) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C24 C23 C22 121.5(4) . .
C24 C23 H23 119.2 . .
C22 C23 H23 119.2 . .
C21 C26 C25 118.3(4) . .
C21 C26 H26 120.9 . .
C25 C26 H26 120.9 . .
C23 C22 C21 120.7(4) . .
C23 C22 H22 119.7 . .
C21 C22 H22 119.7 . .
C23 C24 C25 120.0(4) . .
C23 C24 H24 120.0 . .
C25 C24 H24 120.0 . .
C22 C21 C26 119.0(4) . .
C22 C21 H21 120.5 . .
C26 C21 H21 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 N11 1.9943(17) 3_665
Mo1 N11 1.9943(17) .
Mo1 N11 1.9943(17) 2_655
Mo1 S20 2.4190(6) .
Mo1 S20 2.4191(5) 2_655
Mo1 S20 2.4191(5) 3_665
S20 C13 1.722(2) .
N12 C13 1.329(2) .
N12 N11 1.343(2) .
O150 C15 1.362(2) .
O150 H150 0.839(17) .
N11 H11 0.8600 .
C13 C14 1.469(3) .
C14 C19 1.406(3) .
C14 C15 1.412(3) .
C15 C16 1.387(3) .
C16 C17 1.381(3) .
C16 H16 0.9300 .
C19 C18 1.381(3) .
C19 H19 0.9300 .
C17 C18 1.392(3) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C25 C24 1.348(6) .
C25 C26 1.382(6) .
C25 H25 0.9300 .
C23 C24 1.323(6) .
C23 C22 1.327(7) .
C23 H23 0.9300 .
C26 C21 1.374(6) .
C26 H26 0.9300 .
C22 C21 1.367(6) .
C22 H22 0.9300 .
C24 H24 0.9300 .
C21 H21 0.9300 .
