#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/85/4318567.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_4318567
loop_
_publ_author_name
'Graeme A. Horley'
'Mary F. Mahon'
'Kieran C. Molloy'
'Peter W. Haycock'
'Christopher P. Myers'
_publ_section_title
;
 Synthesis and Characterization of Novel Homoleptic N,N-Dialkylcarbamato
 Complexes of Antimony: Precursors for the Deposition of Antimony Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5052
_journal_page_last               5058
_journal_paper_doi               10.1021/ic0202716
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C9 H18 N3 O6 Sb'
_chemical_formula_weight         386.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.029(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7520(5)
_cell_length_b                   14.2970(8)
_cell_length_c                   11.8150(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1405.79(14)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14053
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  1.02
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.776
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0410P)²+2.4436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                3188
_reflns_number_total             3855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202716_1.cif
_cod_data_source_block           k01kcm6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Multi-Scan'
changed to 'multi-scan' 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 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4318567
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, 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
Sb1 Sb 0.425591(18) 0.066100(12) 0.814841(13) 0.02006(8) Uani 1 1 d . . .
O1 O 0.2711(2) -0.03493(13) 0.72302(15) 0.0229(4) Uani 1 1 d . . .
O2 O 0.1319(2) 0.09726(14) 0.70257(16) 0.0272(4) Uani 1 1 d . . .
O3 O 0.4510(2) 0.09509(14) 0.65156(15) 0.0253(4) Uani 1 1 d . . .
O4 O 0.6510(2) 0.17311(15) 0.77944(16) 0.0300(4) Uani 1 1 d . . .
O5 O 0.5844(2) -0.04097(14) 0.83190(16) 0.0271(4) Uani 1 1 d . . .
O6 O 0.6962(2) 0.01374(14) 1.01757(15) 0.0256(4) Uani 1 1 d . . .
N1 N 0.0005(3) -0.03949(18) 0.6361(2) 0.0281(5) Uani 1 1 d . . .
N2 N 0.6043(3) 0.19104(16) 0.57934(19) 0.0250(5) Uani 1 1 d . . .
N3 N 0.8142(3) -0.10564(17) 0.94744(19) 0.0267(5) Uani 1 1 d . . .
C1 C 0.1326(3) 0.0106(2) 0.6874(2) 0.0237(5) Uani 1 1 d . . .
C2 C 0.0051(4) -0.1387(2) 0.6095(3) 0.0335(6) Uani 1 1 d . . .
H2A H 0.1166 -0.1606 0.6365 0.050 Uiso 1 1 calc R . .
H2B H -0.0402 -0.1484 0.5235 0.050 Uiso 1 1 calc R . .
H2C H -0.0582 -0.1737 0.6507 0.050 Uiso 1 1 calc R . .
C3 C -0.1568(3) 0.0058(2) 0.6020(3) 0.0356(7) Uani 1 1 d . . .
H3A H -0.2118 -0.0096 0.6603 0.053 Uiso 1 1 calc R . .
H3B H -0.2210 -0.0164 0.5232 0.053 Uiso 1 1 calc R . .
H3C H -0.1430 0.0737 0.5997 0.053 Uiso 1 1 calc R . .
C4 C 0.5727(3) 0.1542(2) 0.6740(2) 0.0230(5) Uani 1 1 d . . .
C5 C 0.7326(4) 0.2602(2) 0.5977(3) 0.0358(7) Uani 1 1 d . . .
H5A H 0.7075 0.3149 0.6388 0.054 Uiso 1 1 calc R . .
H5B H 0.7420 0.2794 0.5205 0.054 Uiso 1 1 calc R . .
H5C H 0.8344 0.2327 0.6462 0.054 Uiso 1 1 calc R . .
C6 C 0.5107(4) 0.1653(2) 0.4584(2) 0.0351(7) Uani 1 1 d . . .
H6A H 0.4891 0.0979 0.4548 0.053 Uiso 1 1 calc R . .
H6B H 0.5713 0.1811 0.4038 0.053 Uiso 1 1 calc R . .
H6C H 0.4087 0.1996 0.4353 0.053 Uiso 1 1 calc R . .
C7 C 0.6979(3) -0.0416(2) 0.9361(2) 0.0223(5) Uani 1 1 d . . .
C8 C 0.9537(3) -0.1081(2) 1.0538(2) 0.0307(6) Uani 1 1 d . . .
H8A H 0.9655 -0.0475 1.0944 0.046 Uiso 1 1 calc R . .
H8B H 1.0503 -0.1213 1.0313 0.046 Uiso 1 1 calc R . .
H8C H 0.9392 -0.1573 1.1074 0.046 Uiso 1 1 calc R . .
C9 C 0.8068(5) -0.1749(3) 0.8561(3) 0.0548(11) Uani 1 1 d . . .
H9A H 0.7987 -0.2375 0.8875 0.082 Uiso 1 1 calc R . .
H9B H 0.9042 -0.1710 0.8321 0.082 Uiso 1 1 calc R . .
H9C H 0.7124 -0.1630 0.7870 0.082 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'
Sb Sb -0.5866 1.5461 '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
O5 Sb1 O1 80.83(7) . . ?
O5 Sb1 O3 88.61(8) . . ?
O1 Sb1 O3 83.69(7) . . ?
O5 Sb1 O2 137.15(7) . . ?
O1 Sb1 O2 56.70(7) . . ?
O3 Sb1 O2 81.96(7) . . ?
O5 Sb1 C1 109.93(8) . . ?
O1 Sb1 C1 29.11(8) . . ?
O3 Sb1 C1 83.91(7) . . ?
O2 Sb1 C1 27.72(8) . . ?
C1 O1 Sb1 102.18(16) . . ?
C1 O2 Sb1 81.50(14) . . ?
C4 O3 Sb1 104.85(14) . . ?
C7 O5 Sb1 112.99(16) . . ?
C1 N1 C2 122.9(2) . . ?
C1 N1 C3 119.8(3) . . ?
C2 N1 C3 117.3(2) . . ?
C4 N2 C6 121.3(2) . . ?
C4 N2 C5 119.3(2) . . ?
C6 N2 C5 119.3(2) . . ?
C7 N3 C9 122.2(2) . . ?
C7 N3 C8 120.6(2) . . ?
C9 N3 C8 117.3(2) . . ?
O2 C1 O1 119.1(2) . . ?
O2 C1 N1 123.6(2) . . ?
O1 C1 N1 117.3(3) . . ?
O2 C1 Sb1 70.78(14) . . ?
O1 C1 Sb1 48.71(12) . . ?
N1 C1 Sb1 164.6(2) . . ?
O4 C4 O3 119.8(2) . . ?
O4 C4 N2 123.7(2) . . ?
O3 C4 N2 116.5(2) . . ?
O6 C7 O5 121.9(2) . . ?
O6 C7 N3 122.9(2) . . ?
O5 C7 N3 115.1(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
Sb1 O5 2.0353(19) . ?
Sb1 O1 2.0454(18) . ?
Sb1 O3 2.0513(18) . ?
Sb1 O2 2.5406(19) . ?
Sb1 C1 2.661(3) . ?
O1 C1 1.325(3) . ?
O2 C1 1.252(4) . ?
O3 C4 1.321(3) . ?
O4 C4 1.252(3) . ?
O5 C7 1.322(3) . ?
O6 C7 1.249(3) . ?
N1 C1 1.336(4) . ?
N1 C2 1.455(4) . ?
N1 C3 1.460(4) . ?
N2 C4 1.340(3) . ?
N2 C6 1.457(3) . ?
N2 C5 1.461(3) . ?
N3 C7 1.345(3) . ?
N3 C9 1.451(4) . ?
N3 C8 1.457(3) . ?
