#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/42/2004203.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004203
loop_
_publ_author_name
'Satake, K.'
'Hattori, T.'
'Kimura, M.'
'Kashino, S.'
_publ_section_title
N-Acetyl-3,6-di-tert-butyl-2-(3,6-di-tert-butyl-3H-azepin-2-yl)-2,3-dihydro-1H-azepine
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2707
_journal_page_last               2710
_journal_paper_doi               10.1107/S0108270195008833
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C30 H48 N2 O'
_chemical_formula_weight         452.7
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 95.48(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.421(8)
_cell_length_b                   12.670(7)
_cell_length_c                   18.450(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     2890(3)
_computing_cell_refinement       'Rigaku AFC Software'
_computing_data_collection
'Rigaku AFC Software (Rigaku Corporation , 1990)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1985)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'MITHRIL (Gilmore, 1984)'
_diffrn_measurement_device       'Rigaku AFC-5R'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5352
_diffrn_reflns_theta_max         26.0
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.15
_refine_ls_extinction_coef       1.09E-6
_refine_ls_extinction_method     'Icorr = Iₒ(1+gIc)'
_refine_ls_goodness_of_fit_obs   1.33
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     443
_refine_ls_number_reflns         2046
_refine_ls_R_factor_obs          0.047
_refine_ls_shift/esd_max         0.37
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/σ²(F)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.030
_reflns_number_observed          2046
_reflns_number_total             5091
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            as1196.cif
_cod_data_source_block           as1196a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value ' w=1/\s^2^(F)' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2004203
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,z
-x,-y,-z
1/2-x,1/2+y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
O(1) 0.5346(2) 0.1358(2) 0.1001(1) 4.5(2)
N(1) 0.6921(2) 0.0605(2) 0.1475(1) 2.5(1)
N(2) 0.7027(2) 0.1585(2) 0.2736(2) 3.1(2)
C(1) 0.7404(3) -0.0265(3) 0.1851(2) 2.9(2)
C(2) 0.8442(3) -0.0456(3) 0.2039(2) 2.9(2)
C(3) 0.9352(3) 0.0190(3) 0.1844(2) 3.6(2)
C(4) 0.9374(3) 0.1057(3) 0.1438(2) 3.4(2)
C(5) 0.8449(3) 0.1663(3) 0.1069(2) 2.7(2)
C(6) 0.7466(3) 0.1635(3) 0.1511(2) 2.4(2)
C(7) 0.7662(3) 0.1995(3) 0.2317(2) 2.5(2)
C(8) 0.8553(3) 0.2795(3) 0.2530(2) 2.7(2)
C(9) 0.9282(3) 0.2294(3) 0.3130(2) 3.2(2)
C(10) 0.9016(3) 0.1870(3) 0.3741(2) 3.6(2)
C(11) 0.7948(3) 0.1730(3) 0.3977(2) 3.4(2)
C(12) 0.7079(3) 0.1673(3) 0.3493(2) 3.6(2)
C(13) 0.5854(3) 0.0567(3) 0.1188(2) 3.2(2)
C(14) 0.5348(4) -0.0505(4) 0.1077(3) 4.8(3)
C(15) 0.8763(3) -0.1421(3) 0.2518(2) 4.0(2)
C(16) 0.7802(5) -0.2117(4) 0.2656(3) 6.8(4)
C(17) 0.9556(4) -0.2117(4) 0.2148(3) 6.7(3)
C(18) 0.9285(5) -0.1033(4) 0.3255(3) 7.1(4)
C(19) 0.8240(3) 0.1417(3) 0.0237(2) 3.4(2)
C(20) 0.9282(4) 0.1658(4) -0.0108(2) 4.8(3)
C(21) 0.7351(4) 0.2129(4) -0.0104(3) 5.4(3)
C(22) 0.7958(4) 0.0254(4) 0.0072(3) 4.8(3)
C(23) 0.8191(3) 0.3959(3) 0.2649(2) 3.3(2)
C(24) 0.9204(4) 0.4594(4) 0.2904(3) 4.9(3)
C(25) 0.7368(4) 0.4099(4) 0.3204(3) 5.1(3)
C(26) 0.7704(4) 0.4382(4) 0.1918(3) 4.8(3)
C(27) 0.7855(4) 0.1588(4) 0.4794(2) 5.3(3)
C(28) 0.8438(5) 0.0559(6) 0.5053(3) 8.8(4)
C(29) 0.8440(5) 0.2514(7) 0.5206(3) 9.0(5)
C(30) 0.6701(6) 0.1574(7) 0.4987(3) 10.4(5)
H(1) 0.685(2) -0.078(2) 0.199(2) 2.9
H(3) 1.007(2) -0.007(2) 0.205(2) 3.6
H(4) 1.007(2) 0.134(2) 0.137(2) 3.4
H(5) 0.870(2) 0.241(2) 0.107(1) 2.7
H(6) 0.690(2) 0.214(2) 0.130(1) 2.4
H(8) 0.900(2) 0.289(2) 0.211(1) 2.6
H(9) 1.003(2) 0.227(2) 0.303(2) 3.2
H(10) 0.960(2) 0.161(2) 0.406(2) 3.6
H(12) 0.636(2) 0.154(2) 0.365(2) 3.6
H(141) 0.580(3) -0.098(3) 0.086(2) 4.8
H(142) 0.505(3) -0.074(3) 0.148(2) 4.8
H(143) 0.468(3) -0.044(3) 0.080(2) 4.8
H(161) 0.741(3) -0.239(3) 0.219(2) 6.7
H(162) 0.725(3) -0.167(3) 0.293(2) 6.7
H(163) 0.806(3) -0.269(3) 0.296(2) 6.7
H(171) 0.968(3) -0.276(3) 0.250(2) 6.7
H(172) 0.916(3) -0.245(3) 0.165(2) 6.7
H(173) 1.024(3) -0.175(3) 0.217(2) 6.7
H(181) 0.942(3) -0.164(3) 0.355(2) 7.1
H(182) 0.860(3) -0.063(3) 0.349(2) 7.1
H(183) 0.991(3) -0.065(3) 0.319(2) 7.1
H(201) 0.919(2) 0.158(3) -0.063(2) 4.8
H(202) 0.994(3) 0.121(3) 0.008(2) 4.8
H(203) 0.955(3) 0.241(3) 0.000(2) 4.8
H(211) 0.753(3) 0.287(3) -0.001(2) 5.4
H(212) 0.726(3) 0.202(3) -0.061(2) 5.4
H(213) 0.656(3) 0.195(3) 0.005(2) 5.4
H(221) 0.843(3) -0.020(3) 0.035(2) 4.8
H(222) 0.716(3) 0.012(3) 0.014(2) 4.8
H(223) 0.797(2) 0.011(3) -0.046(2) 4.8
H(241) 0.892(3) 0.534(3) 0.292(2) 4.9
H(242) 0.947(3) 0.440(3) 0.340(2) 4.9
H(243) 0.978(3) 0.452(3) 0.256(2) 4.9
H(251) 0.674(3) 0.375(3) 0.304(2) 5.1
H(252) 0.724(3) 0.483(3) 0.326(2) 5.1
H(253) 0.767(3) 0.388(3) 0.371(2) 5.1
H(261) 0.755(3) 0.512(3) 0.196(2) 4.8
H(262) 0.704(3) 0.396(3) 0.174(2) 4.8
H(263) 0.828(3) 0.435(3) 0.154(2) 4.8
H(281) 0.832(3) 0.046(3) 0.557(2) 8.8
H(282) 0.919(3) 0.070(4) 0.504(2) 8.8
H(283) 0.779(4) 0.007(4) 0.481(2) 8.8
H(291) 0.792(4) 0.317(4) 0.507(2) 9.0
H(292) 0.906(4) 0.249(5) 0.514(3) 9.0
H(293) 0.838(3) 0.238(3) 0.577(2) 9.0
H(301) 0.631(4) 0.224(4) 0.480(3) 10.4
H(302) 0.647(5) 0.085(4) 0.484(3) 10.4
H(303) 0.671(3) 0.145(4) 0.550(2) 10.4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) C(1) C(2) 129.1(4) yes
C(1) N(1) C(6) 120.1(3) yes
C(1) C(2) C(3) 125.9(4) yes
C(2) C(3) C(4) 131.0(4) yes
C(3) C(4) C(5) 128.7(4) yes
C(4) C(5) C(6) 111.4(3) yes
N(1) C(6) C(5) 112.5(3) yes
N(2) C(12) C(11) 129.1(4) yes
C(7) N(2) C(12) 127.2(3) yes
N(2) C(7) C(8) 126.5(3) yes
C(7) C(8) C(9) 106.3(3) yes
C(8) C(9) C(10) 128.2(4) yes
C(9) C(10) C(11) 128.3(4) yes
C(10) C(11) C(12) 120.7(4) yes
C(12) C(11) C(27) 121.3(4) yes
C(16) C(15) C(17) 106.7(4) no
C(16) C(15) C(18) 108.0(4) no
C(17) C(15) C(18) 110.2(4) no
C(5) C(19) C(22) 113.5(3) no
N(1) C(6) C(7) 109.5(3) yes
C(20) C(19) C(21) 108.6(4) no
C(5) C(6) C(7) 116.3(3) yes
C(20) C(19) C(22) 107.2(4) no
N(2) C(7) C(6) 114.5(3) yes
C(21) C(19) C(22) 110.1(4) no
C(8) C(23) C(24) 107.4(3) no
C(6) C(7) C(8) 119.1(3) yes
C(8) C(23) C(25) 115.1(3) no
O(1) C(13) N(1) 122.2(4) yes
O(1) C(13) C(14) 120.5(4) yes
N(1) C(13) C(14) 117.2(4) yes
C(1) N(1) C(13) 120.7(3) yes
C(1) C(2) C(15) 119.2(4) yes
C(2) C(15) C(16) 113.0(4) no
C(2) C(15) C(17) 110.2(4) no
C(2) C(15) C(18) 108.6(4) no
C(3) C(2) C(15) 114.9(3) yes
C(4) C(5) C(19) 113.2(3) yes
C(5) C(19) C(20) 107.6(3) no
C(5) C(19) C(21) 109.6(3) no
C(6) N(1) C(13) 118.0(3) yes
C(6) C(5) C(19) 116.8(3) yes
C(8) C(23) C(26) 107.7(3) no
C(7) C(8) C(23) 116.8(3) yes
C(24) C(23) C(25) 108.5(4) no
C(9) C(8) C(23) 117.2(3) yes
C(24) C(23) C(26) 109.4(4) no
C(25) C(23) C(26) 108.6(4) no
C(11) C(27) C(28) 109.1(4) no
C(11) C(27) C(29) 108.6(4) no
C(10) C(11) C(27) 117.9(4) yes
C(11) C(27) C(30) 113.2(4) no
C(28) C(27) C(29) 107.8(5) no
C(28) C(27) C(30) 110.2(5) no
C(29) C(27) C(30) 107.8(5) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
N(1) C(1) 1.406(4) yes
N(1) C(6) 1.469(4) yes
C(1) C(2) 1.326(5) yes
C(2) C(3) 1.468(5) yes
C(3) C(4) 1.331(5) yes
C(4) C(5) 1.490(5) yes
C(5) C(6) 1.532(5) yes
N(2) C(7) 1.267(4) yes
N(2) C(12) 1.396(4) yes
C(7) C(8) 1.525(5) yes
C(8) C(9) 1.502(5) yes
C(9) C(10) 1.320(5) yes
C(10) C(11) 1.446(5) yes
C(11) C(12) 1.336(5) yes
C(6) C(7) 1.552(4) yes
N(1) C(13) 1.380(4) yes
O(1) C(13) 1.217(4) yes
C(2) C(15) 1.538(5) no
C(5) C(19) 1.563(5) no
C(8) C(23) 1.563(5) no
C(11) C(27) 1.533(5) no
C(13) C(14) 1.502(6) yes
C(15) C(16) 1.525(6) no
C(15) C(17) 1.530(6) no
C(15) C(18) 1.530(6) no
C(19) C(20) 1.528(6) no
C(19) C(21) 1.516(6) no
C(19) C(22) 1.538(6) no
C(23) C(24) 1.530(5) no
C(23) C(25) 1.525(6) no
C(23) C(26) 1.521(5) no
C(27) C(28) 1.544(8) no
C(27) C(29) 1.542(9) no
C(27) C(30) 1.510(8) no
C(1) H(1) 0.99(3) no
C(3) H(3) 0.99(3) no
C(4) H(4) 0.96(3) no
C(5) H(5) 0.99(3) no
C(6) H(6) 1.00(3) no
C(8) H(8) 1.00(3) no
C(9) H(9) 0.96(3) no
C(10) H(10) 0.95(3) no
C(12) H(12) 0.98(3) no
C(14) H(141) 0.94(3) no
C(14) H(142) 0.91(3) no
C(14) H(143) 0.93(3) no
C(16) H(161) 1.00(3) no
C(16) H(162) 1.06(3) no
C(16) H(163) 0.96(4) no
C(17) H(171) 1.04(3) no
C(17) H(172) 1.09(3) no
C(17) H(173) 0.97(3) no
C(18) H(181) 0.95(4) no
C(18) H(182) 1.12(3) no
C(18) H(183) 0.94(4) no
C(20) H(201) 0.97(3) no
C(20) H(202) 1.02(3) no
C(20) H(203) 1.02(3) no
C(21) H(211) 0.98(3) no
C(21) H(212) 0.93(3) no
C(21) H(213) 1.07(3) no
C(22) H(221) 0.94(3) no
C(22) H(222) 1.03(3) no
C(22) H(223) 1.01(3) no
C(24) H(241) 1.01(3) no
C(24) H(242) 0.98(3) no
C(24) H(243) 1.00(3) no
C(25) H(251) 0.92(3) no
C(25) H(252) 0.95(3) no
C(25) H(253) 1.01(3) no
C(26) H(261) 0.95(3) no
C(26) H(262) 1.01(3) no
C(26) H(263) 1.05(3) no
C(28) H(281) 0.99(4) no
C(28) H(282) 0.95(4) no
C(28) H(283) 1.07(4) no
C(29) H(291) 1.07(4) no
C(29) H(292) 0.79(5) no
C(29) H(293) 1.07(4) no
C(30) H(301) 1.02(4) no
C(30) H(302) 0.99(5) no
C(30) H(303) 0.96(4) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
C(3) C(4) C(5) C(6) 33.4(6) yes
N(1) C(1) C(2) C(3) -4.6(6) yes
N(1) C(6) C(5) C(4) -73.5(4) yes
N(2) C(7) C(6) C(5) -152.6(3) yes
C(5) C(6) C(7) C(8) 28.4(5) yes
N(2) C(7) C(8) C(9) 56.8(5) yes
N(2) C(12) C(11) C(10) 9.8(7) yes
C(1) N(1) C(6) C(5) 72.9(4) yes
C(1) N(1) C(6) C(7) -58.1(4) yes
C(1) C(2) C(3) C(4) -2.2(7) yes
C(7) N(2) C(12) C(11) -35.0(7) yes
C(7) C(8) C(9) C(10) -52.5(5) yes
C(2) C(1) N(1) C(6) -27.0(6) yes
C(2) C(3) C(4) C(5) 2.2(7) yes
C(8) C(7) N(2) C(12) -8.2(6) yes
C(8) C(9) C(10) C(11) 3.4(7) yes
C(9) C(10) C(11) C(12) 24.5(7) yes
C(1) N(1) C(13) O(1) 163.8(4) yes
