#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:45:54 +0100 (vie 25 de mar de 2016) $
#$Revision: 179763 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/59/7005966.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_7005966
loop_
_publ_author_name
'Cotton, F. Albert'
'Murillo, Carlos A.'
'Wang, Xiaoping'
'Wilkinson, Chad C.'
_publ_section_title
;
 Increasing the solubility of strong reducing agents containing
 Mo(2)(4+) units and alkyl-substituted guanidinate ligands.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3943
_journal_page_last               3951
_journal_paper_doi               10.1039/b707201e
_journal_year                    2007
_chemical_formula_moiety         'C14 H32 Cl N3 O3'
_chemical_formula_sum            'C14 H32 Cl N3 O3'
_chemical_formula_weight         325.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   12.5762(9)
_cell_length_b                   21.295(4)
_cell_length_c                   6.6890(7)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.815
_cell_measurement_theta_min      9.085
_cell_volume                     1791.4(4)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius FAST'
_diffrn_measurement_method       ω-scans
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9093
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.9707
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0519P)²+1.0837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                1556
_reflns_number_total             1673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b707201e.txt
_cod_data_source_block           SIIIHCL
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7005966
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.64553(4) 0.2500 0.10337(8) 0.0281(2) Uani 1 2 d S . .
N1 N 0.87788(14) 0.2500 0.8360(3) 0.0188(4) Uani 1 2 d S . .
H1A H 0.8158 0.2500 0.7662 0.023 Uiso 1 2 calc SR . .
H1E H 0.8621 0.2500 0.9688 0.023 Uiso 1 2 calc SR . .
O1 O 0.67369(10) 0.34898(6) 0.43865(19) 0.0332(3) Uani 1 1 d . . .
H1B H 0.6587 0.3198 0.3612 0.050 Uiso 1 1 calc R . .
N2 N 0.76501(11) 0.33305(7) 0.5495(2) 0.0258(3) Uani 1 1 d . . .
C1 C 0.94182(12) 0.30738(6) 0.7844(2) 0.0204(3) Uani 1 1 d . . .
H1C H 0.9659 0.3034 0.6456 0.024 Uiso 1 1 calc R . .
H1D H 1.0053 0.3080 0.8692 0.024 Uiso 1 1 calc R . .
C4 C 0.84893(15) 0.38069(8) 1.0259(3) 0.0282(4) Uani 1 1 d . . .
H4A H 0.7915 0.3510 1.0551 0.034 Uiso 1 1 calc R . .
H4B H 0.9087 0.3702 1.1139 0.034 Uiso 1 1 calc R . .
C6 C 0.96707(14) 0.42168(8) 0.7487(3) 0.0285(4) Uani 1 1 d . . .
H6A H 0.9322 0.4628 0.7564 0.034 Uiso 1 1 calc R . .
H6B H 1.0244 0.4214 0.8479 0.034 Uiso 1 1 calc R . .
C3 C 0.79031(12) 0.37584(7) 0.6700(2) 0.0236(4) Uani 1 1 d . . .
H3A H 0.7487 0.4125 0.6748 0.028 Uiso 1 1 calc R . .
C2 C 0.88486(12) 0.37049(7) 0.8069(2) 0.0205(3) Uani 1 1 d . . .
C7 C 1.01636(16) 0.41491(9) 0.5420(3) 0.0404(5) Uani 1 1 d . . .
H7A H 1.0667 0.4487 0.5200 0.061 Uiso 1 1 calc R . .
H7B H 0.9609 0.4168 0.4414 0.061 Uiso 1 1 calc R . .
H7C H 1.0529 0.3749 0.5329 0.061 Uiso 1 1 calc R . .
C5 C 0.81033(16) 0.44653(8) 1.0792(3) 0.0355(4) Uani 1 1 d . . .
H5A H 0.7896 0.4477 1.2188 0.053 Uiso 1 1 calc R . .
H5B H 0.7497 0.4573 0.9963 0.053 Uiso 1 1 calc R . .
H5C H 0.8671 0.4765 1.0564 0.053 Uiso 1 1 calc R . .
O2 O 0.90984(14) 0.2500 0.2485(2) 0.0328(4) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0226(3) 0.0340(3) 0.0277(3) 0.000 -0.0041(2) 0.000
N1 0.0217(9) 0.0160(9) 0.0187(9) 0.000 0.0020(7) 0.000
O1 0.0267(6) 0.0427(7) 0.0302(6) -0.0072(5) -0.0090(5) 0.0058(5)
N2 0.0223(7) 0.0277(7) 0.0273(7) -0.0019(6) -0.0047(5) 0.0019(6)
C1 0.0202(7) 0.0182(8) 0.0227(8) -0.0005(6) 0.0008(6) -0.0024(6)
C4 0.0402(10) 0.0219(8) 0.0225(9) -0.0026(6) 0.0016(7) 0.0014(7)
C6 0.0285(9) 0.0198(8) 0.0372(9) 0.0034(7) -0.0018(7) -0.0045(7)
C3 0.0232(8) 0.0215(8) 0.0261(8) -0.0013(6) 0.0007(6) 0.0037(6)
C2 0.0238(8) 0.0171(8) 0.0205(8) -0.0003(6) 0.0000(6) -0.0010(6)
C7 0.0389(11) 0.0306(9) 0.0517(12) 0.0103(9) 0.0168(9) -0.0028(8)
C5 0.0450(11) 0.0275(9) 0.0340(9) -0.0096(7) 0.0041(8) 0.0029(8)
O2 0.0308(9) 0.0442(10) 0.0235(9) 0.000 -0.0015(7) 0.000
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'
Cl Cl 0.1484 0.1585 '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
C1 N1 C1 108.77(16) . 7_565 ?
N2 O1 Cl1 108.08(9) . . ?
C3 N2 O1 111.67(13) . . ?
N1 C1 C2 116.16(13) . . ?
C5 C4 C2 116.27(14) . . ?
C7 C6 C2 115.64(14) . . ?
N2 C3 C2 122.35(15) . . ?
C3 C2 C1 112.11(13) . . ?
C3 C2 C4 109.54(13) . . ?
C1 C2 C4 110.67(13) . . ?
C3 C2 C6 108.69(13) . . ?
C1 C2 C6 106.28(13) . . ?
C4 C2 C6 109.46(13) . . ?
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
Cl1 O1 3.0981(13) . ?
N1 C1 1.5030(17) . ?
N1 C1 1.5030(17) 7_565 ?
O1 N2 1.4085(18) . ?
N2 C3 1.258(2) . ?
C1 C2 1.530(2) . ?
C4 C5 1.526(2) . ?
C4 C2 1.549(2) . ?
C6 C7 1.522(3) . ?
C6 C2 1.552(2) . ?
C3 C2 1.505(2) . ?
