#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/18/4071838.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_4071838
loop_
_publ_author_name
'Abernethy, Robyn J.'
'Foreman, Mark R. St.-J.'
'Hill, Anthony F.'
'Tshabang, Never'
'Willis, Anthony C.'
'Young, Rowan D.'
_publ_section_title
;
 Poly(methimazolyl)borato Nitrosyl Complexes of Molybdenum and Tungsten
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4455
_journal_paper_doi               10.1021/om800416j
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        local
_chemical_formula_moiety         'C10 H12 B Mo N5 O3 S2, 0.5(C2 H6 O)'
_chemical_formula_sum            'C11 H15 B Mo N5 O3.5 S2'
_chemical_formula_weight         444.15
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-04-15
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2003-06    - data collected and early structure done
2008-04-15 - Report on C11 H15 B Mo N5 O3.50 S2 
            by Anthony C. Willis
            for   Anthony F. Hill and Never Tshabang

2008-04-17 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4413(6)
_cell_length_b                   6.7479(2)
_cell_length_c                   15.0143(6)
_cell_measurement_reflns_used    10203
_cell_measurement_temperature    200
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1767.07(11)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20383
_diffrn_reflns_theta_full        27.487
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         2.713
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1528
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1227
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.006567
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, 
(Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.294 0.186 0.115 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0711
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0377
_reflns_limit_h_max              22
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                1227
_reflns_number_total             2104
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.88
_oxford_diffrn_Wilson_scale      47.59
_oxford_refine_ls_scale          0.1528(4)
_oxford_structure_analysis_title 'transformed for std setting'
_cod_data_source_file            om800416j-file002.cif
_cod_data_source_block           hil0301
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_sg_symbol_H-M      'P n n m '
_cod_original_formula_sum        'C11 H15 B Mo N5 O3.50 S2'
_cod_database_code               4071838
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mo1 Mo 0.35038(2) 0.58131(7) 0.5000 0.0337 1.0000 Uani S T
S1 S 0.25574(7) 0.48168(17) 0.38110(9) 0.0553 1.0000 Uani . .
O1 O 0.4208(2) 0.1524(6) 0.5000 0.0440 1.0000 Uani S T
O2 O 0.46546(16) 0.7086(4) 0.35578(19) 0.0461 1.0000 Uani . .
O51 O 0.0890(6) 0.3782(17) 0.5000 0.1062 0.5 Uani DS T
N2 N 0.42073(19) 0.6597(5) 0.4101(2) 0.0350 0.5 Uani . .
N11 N 0.19628(17) 0.8520(5) 0.4151(2) 0.0351 1.0000 Uani . .
N12 N 0.1473(2) 0.6991(5) 0.2997(2) 0.0447 1.0000 Uani . .
C1 C 0.3951(3) 0.3068(8) 0.5000 0.0362 1.0000 Uani S T
C2 C 0.42073(19) 0.6597(5) 0.4101(2) 0.0350 0.5 Uani . .
C11 C 0.1992(2) 0.6844(6) 0.3659(2) 0.0353 1.0000 Uani . .
C12 C 0.1408(3) 0.9744(7) 0.3769(3) 0.0525 1.0000 Uani . .
C13 C 0.1106(3) 0.8804(7) 0.3070(3) 0.0610 1.0000 Uani . .
C14 C 0.1342(3) 0.5527(7) 0.2305(3) 0.0656 1.0000 Uani . .
C52 C 0.0456(10) 0.544(3) 0.5000 0.1336 0.5 Uani DS T
C53 C -0.0355(11) 0.518(5) 0.5000 0.1336 0.5 Uani DS T
B1 B 0.2402(3) 0.9098(9) 0.5000 0.0320 1.0000 Uani S T
H1 H 0.299(3) 0.838(8) 0.5000 0.030(13) 1.0000 Uiso S .
H2 H 0.250(3) 1.079(8) 0.5000 0.036(15) 1.0000 Uiso S .
H51 H 0.1299 0.4087 0.5000 0.1270 0.5 Uiso R .
H121 H 0.1262 1.1095 0.3983 0.0630 1.0000 Uiso R .
H131 H 0.0691 0.9316 0.2672 0.0733 1.0000 Uiso R .
H141 H 0.0926 0.6001 0.1899 0.0788 1.0000 Uiso R .
H142 H 0.1824 0.5331 0.1956 0.0788 1.0000 Uiso R .
H143 H 0.1185 0.4243 0.2583 0.0788 1.0000 Uiso R .
H521 H 0.0593 0.622 0.5544 0.1603 0.5 Uiso R .
H531 H -0.0614 0.650 0.5000 0.1603 0.5 Uiso R .
H532 H -0.0509 0.442 0.5544 0.1603 0.5 Uiso R .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 8_556 Mo1 N2 8_556 89.64(10) yes
S1 8_556 Mo1 S1 . 90.10(7) yes
N2 8_556 Mo1 S1 . 179.14(10) yes
S1 8_556 Mo1 N2 . 179.14(10) yes
N2 8_556 Mo1 N2 . 90.6(2) yes
S1 . Mo1 N2 . 89.64(10) yes
S1 8_556 Mo1 C1 . 90.48(11) yes
N2 8_556 Mo1 C1 . 90.34(14) yes
S1 . Mo1 C1 . 90.48(11) yes
N2 . Mo1 C1 . 90.34(14) yes
S1 8_556 Mo1 H1 . 86.5(11) yes
N2 8_556 Mo1 H1 . 92.7(11) yes
S1 . Mo1 H1 . 86.5(11) yes
N2 . Mo1 H1 . 92.7(11) yes
C1 . Mo1 H1 . 175.7(16) yes
Mo1 . S1 C11 . 105.07(14) yes
C52 . O51 H51 . 108.0 yes
O2 . N2 Mo1 . 178.6(3) yes
C11 . N11 C12 . 107.3(3) yes
C11 . N11 B1 . 130.3(3) yes
C12 . N11 B1 . 122.4(4) yes
C11 . N12 C13 . 108.4(4) yes
C11 . N12 C14 . 125.7(4) yes
C13 . N12 C14 . 125.8(4) yes
Mo1 . C1 O1 . 179.6(4) yes
S1 . C11 N11 . 128.4(3) yes
S1 . C11 N12 . 123.1(3) yes
N11 . C11 N12 . 108.5(3) yes
N11 . C12 C13 . 108.4(4) yes
N11 . C12 H121 . 125.8 no
C13 . C12 H121 . 125.8 no
N12 . C13 C12 . 107.5(4) yes
N12 . C13 H131 . 126.3 no
C12 . C13 H131 . 126.3 no
N12 . C14 H141 . 109.5 no
N12 . C14 H142 . 109.4 no
H141 . C14 H142 . 109.5 no
N12 . C14 H143 . 109.5 no
H141 . C14 H143 . 109.5 no
H142 . C14 H143 . 109.5 no
H521 8_556 C52 O51 . 107.6 no
H521 8_556 C52 C53 . 107.5 no
O51 . C52 C53 . 116.9(16) yes
H521 8_556 C52 H521 . 109.5 no
O51 . C52 H521 . 107.6 no
C53 . C52 H521 . 107.5 no
H532 8_556 C53 C52 . 109.3 no
H532 8_556 C53 H531 . 109.5 no
C52 . C53 H531 . 109.7 no
H532 8_556 C53 H532 . 109.5 no
C52 . C53 H532 . 109.3 no
H531 . C53 H532 . 109.5 no
N11 . B1 N11 8_556 112.0(4) yes
N11 . B1 H1 . 110.1(13) no
N11 8_556 B1 H1 . 110.1(13) no
N11 . B1 H2 . 109.1(14) no
N11 8_556 B1 H2 . 109.1(14) no
H1 . B1 H2 . 106(4) no
Mo1 . H1 B1 . 142(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 S1 . 2.5225(12) yes
Mo1 N2 . 1.900(4) yes
Mo1 C1 . 2.010(6) yes
Mo1 H1 . 1.95(6) yes
Mo1 S1 8_556 2.5225(12) yes
Mo1 N2 8_556 1.900(4) yes
S1 C11 . 1.702(4) yes
O1 C1 . 1.134(6) yes
O2 N2 . 1.175(4) yes
O51 C53 2_566 1.17(3) yes
O51 C52 . 1.350(10) yes
O51 H51 . 0.743 no
N11 C11 . 1.351(5) yes
N11 C12 . 1.395(5) yes
N11 B1 . 1.538(4) yes
N12 C11 . 1.348(5) yes
N12 C13 . 1.385(6) yes
N12 C14 . 1.451(6) yes
C12 C13 . 1.334(7) yes
C12 H121 . 1.000 no
C13 H131 . 1.000 no
C14 H141 . 1.000 no
C14 H142 . 1.000 no
C14 H143 . 1.000 no
C52 C53 . 1.425(9) yes
C52 H521 . 1.000 no
C52 H521 8_556 1.000 no
C53 H531 . 1.000 no
C53 H532 . 1.000 no
C53 H532 8_556 1.000 no
B1 H1 . 1.14(5) no
B1 H2 . 1.16(5) no
