#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/16/2011654.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_2011654
loop_
_publ_author_name
'Ohba, Shigeru'
'Eishima, Makoto'
'Seki, Hiroshi'
_publ_section_title
;
 Aquanitro(α,β,γ,δ-tetraphenylporphyrinato)cobalt(III)
 N,N-dimethylformamide disolvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e555
_journal_page_last               e556
_journal_paper_doi               10.1107/S0108270100015109
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Co (C44 H28 N4) (H2 O) (N O2)], 2C3 H7 N O'
_chemical_formula_moiety         'C44 H30 Co N5 O3, 2C3 H7 N O'
_chemical_formula_structural     '[Co (C44 H28 N4) (H2 O) (N O2)], 2C3 H7 N O'
_chemical_formula_sum            'C50 H44 Co N7 O5'
_chemical_formula_weight         881.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                105.060(10)
_cell_angle_beta                 97.470(10)
_cell_angle_gamma                107.580(10)
_cell_formula_units_Z            1
_cell_length_a                   10.3550(10)
_cell_length_b                   11.815(2)
_cell_length_c                   9.9000(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      13.7
_cell_volume                     1086.0(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
;TEXSAN
(Molecular Structure Corporation, 1999)
;
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .016
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5271
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .453
_exptl_absorpt_correction_T_max  .928
_exptl_absorpt_correction_T_min  .900
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .15
_refine_diff_density_max         .33
_refine_diff_density_min         -.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4996
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.0567P)²+0.3931P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .123
_reflns_number_gt                3676
_reflns_number_total             4996
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0451.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C50 H44 Co N7 O5 '
_cod_database_code               2011654
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Co1 .0000 .0000 .0000 .04300(10) Uani d S 1.00 . . Co
O2 -.2505(4) -.2009(4) -.0530(5) .0790(10) Uani d P .50 . . O
O3 -.2073(5) -.0713(4) .1512(6) .0900(10) Uani d P .50 . . O
O4 -.1700(2) -.1054(2) .0363(2) .0493(4) Uani d P .50 . . O
O5 .3833(5) .2416(5) .2027(5) .0880(10) Uani d P .50 . . O
O6 -.6745(5) -.0083(5) -.1683(6) .104(2) Uani d P .50 . . O
N7 -.1700(2) -.1054(2) .0363(2) .0493(4) Uani d P .50 . . N
N8 -.1103(2) .0033(2) -.1775(2) .0445(4) Uani d . 1.00 . . N
N9 .0276(2) -.1532(2) -.1108(2) .0421(4) Uani d . 1.00 . . N
N10 .5472(9) .1796(7) .3089(7) .073(2) Uani d P .50 . . N
N11 -.6330(10) -.1629(7) -.3225(8) .078(2) Uani d P .50 . . N
C12 -.1431(3) -.0808(2) -.3131(2) .0466(5) Uani d . 1.00 . . C
C13 -.1032(2) -.1845(2) -.3525(2) .0452(5) Uani d . 1.00 . . C
C14 -.0222(2) -.2163(2) -.2555(2) .0447(5) Uani d . 1.00 . . C
C15 .0241(3) -.3209(2) -.2952(3) .0524(6) Uani d . 1.00 . . C
C16 .0998(3) -.3225(2) -.1758(3) .0521(6) Uani d . 1.00 . . C
C17 .1021(2) -.2187(2) -.0598(2) .0440(5) Uani d . 1.00 . . C
C18 .1710(2) -.1901(2) .0804(2) .0448(5) Uani d . 1.00 . . C
C19 .1749(2) -.0876(2) .1904(2) .0468(5) Uani d . 1.00 . . C
C20 .2491(3) -.0543(2) .3359(3) .0561(6) Uani d . 1.00 . . C
C21 .2300(3) .0490(2) .4115(3) .0556(6) Uani d . 1.00 . . C
C22 -.1527(3) -.2682(2) -.5041(2) .0463(5) Uani d . 1.00 . . C
C23 -.1035(3) -.2310(3) -.6150(3) .0632(7) Uani d . 1.00 . . C
C24 -.1517(4) -.3094(4) -.7554(3) .0797(10) Uani d . 1.00 . . C
C25 -.2492(4) -.4250(3) -.7850(3) .0840(10) Uani d . 1.00 . . C
C26 -.3000(4) -.4639(3) -.6791(4) .0793(9) Uani d . 1.00 . . C
C27 -.2524(3) -.3860(2) -.5377(3) .0597(6) Uani d . 1.00 . . C
C28 .2446(2) -.2744(2) .1158(2) .0447(5) Uani d . 1.00 . . C
C29 .3858(3) -.2438(2) .1246(3) .0610(6) Uani d . 1.00 . . C
C30 .4530(3) -.3222(3) .1569(4) .0711(8) Uani d . 1.00 . . C
C31 .3804(3) -.4307(3) .1784(3) .0670(7) Uani d . 1.00 . . C
C32 .2425(3) -.4611(2) .1707(3) .0659(7) Uani d . 1.00 . . C
C33 .1734(3) -.3836(2) .1393(3) .0558(6) Uani d . 1.00 . . C
C34 .4589(9) .1745(7) .1993(8) .068(2) Uani d P .50 . . C
C35 .6220(10) .0960(10) .2920(10) .104(4) Uani d P .50 . . C
C36 .5648(10) .2575(8) .4534(8) .099(2) Uani d P .50 . . C
C37 -.7022(10) -.0881(7) -.2885(8) .078(2) Uani d P .50 . . C
C38 -.6800(10) -.2609(8) -.4602(9) .109(3) Uani d P .50 . . C
C39 -.5240(10) -.1610(10) -.217(2) .110(4) Uani d P .50 . . C
H15 .0045 -.3784 -.3889 .0628 Uiso calc . 1.00 . . H
H16 .1439 -.3813 -.1691 .0623 Uiso calc . 1.00 . . H
H20 .3023 -.0974 .3721 .0670 Uiso calc . 1.00 . . H
H21 .2716 .0857 .5112 .0666 Uiso calc . 1.00 . . H
H23 -.0354 -.1503 -.5943 .0756 Uiso calc . 1.00 . . H
H24 -.1170 -.2827 -.8304 .0956 Uiso calc . 1.00 . . H
H25 -.2821 -.4791 -.8815 .1006 Uiso calc . 1.00 . . H
H26 -.3684 -.5447 -.7016 .0953 Uiso calc . 1.00 . . H
H27 -.2883 -.4137 -.4638 .0714 Uiso calc . 1.00 . . H
H29 .4371 -.1689 .1084 .0730 Uiso calc . 1.00 . . H
H30 .5504 -.2999 .1641 .0851 Uiso calc . 1.00 . . H
H31 .4266 -.4847 .1986 .0803 Uiso calc . 1.00 . . H
H32 .1922 -.5362 .1870 .0789 Uiso calc . 1.00 . . H
H33 .0763 -.4064 .1339 .0669 Uiso calc . 1.00 . . H
H34 .4492 .1164 .1090 .0818 Uiso calc P .50 . . H
H35A .5584 .0124 .2610 .1241 Uiso calc P .50 . . H
H35B .6763 .1082 .2237 .1241 Uiso calc P .50 . . H
H35C .6815 .1117 .3821 .1241 Uiso calc P .50 . . H
H36A .6340 .2469 .5164 .1191 Uiso calc P .50 . . H
H36B .5927 .3431 .4563 .1191 Uiso calc P .50 . . H
H36C .4792 .2355 .4822 .1191 Uiso calc P .50 . . H
H37 -.7774 -.0947 -.3593 .0932 Uiso calc P .50 . . H
H38A -.7707 -.3155 -.4674 .1310 Uiso calc P .50 . . H
H38B -.6806 -.2245 -.5351 .1310 Uiso calc P .50 . . H
H38C -.6181 -.3064 -.4675 .1310 Uiso calc P .50 . . H
H39A -.5592 -.1819 -.1391 .1280 Uiso calc P .50 . . H
H39B -.4832 -.2208 -.2586 .1280 Uiso calc P .50 . . H
H39C -.4532 -.0802 -.1813 .1280 Uiso calc P .50 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C)
;
Co Co .349 .972
;International Tables for Crystallography
(1992, Vol. C)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O4 Co1 O4 . 1_555 2_555 180.0 no
O4 Co1 N8 . 1_555 1_555 90.00(8) no
O4 Co1 N8 . 1_555 2_555 90.00(8) no
O4 Co1 N9 . 1_555 1_555 89.25(7) no
O4 Co1 N9 . 1_555 2_555 90.75(7) no
N7 Co1 N7 . 1_555 2_555 180.0 no
N8 Co1 N8 . 1_555 2_555 180.0 no
N8 Co1 N9 . 1_555 1_555 90.14(8) no
N8 Co1 N9 . 1_555 2_555 89.86(8) no
N9 Co1 N9 . 1_555 2_555 180.0 no
Co1 N7 O2 . 1_555 1_555 123.0(3) no
Co1 N7 O3 . 1_555 1_555 120.9(2) no
O2 N7 O3 . 1_555 1_555 115.8(3) yes
Co1 N8 C12 . 1_555 1_555 127.3(2) no
Co1 N8 C19 . 1_555 2_555 127.40(10) no
C12 N8 C19 . 1_555 2_555 105.2(2) no
Co1 N9 C14 . 1_555 1_555 127.2(2) no
Co1 N9 C17 . 1_555 1_555 127.40(10) no
C14 N9 C17 . 1_555 1_555 105.4(2) no
C34 N10 C35 . 1_555 1_555 119.9(8) no
C34 N10 C36 . 1_555 1_555 123.6(9) no
C35 N10 C36 . 1_555 1_555 116.1(9) no
C37 N11 C38 . 1_555 1_555 120.0(9) no
C37 N11 C39 . 1_555 1_555 120.1(9) no
C38 N11 C39 . 1_555 1_555 119.0(10) no
N8 C12 C13 . 1_555 1_555 126.2(2) no
N8 C12 C21 . 1_555 2_555 110.3(2) no
C13 C12 C21 . 1_555 2_555 123.5(2) no
C12 C13 C14 . 1_555 1_555 122.9(2) no
C12 C13 C22 . 1_555 1_555 118.8(2) no
C14 C13 C22 . 1_555 1_555 118.3(2) no
N9 C14 C13 . 1_555 1_555 126.2(2) no
N9 C14 C15 . 1_555 1_555 110.1(2) no
C13 C14 C15 . 1_555 1_555 123.7(2) no
C14 C15 C16 . 1_555 1_555 107.4(2) no
C14 C15 H15 . 1_555 1_555 126.3 no
C16 C15 H15 . 1_555 1_555 126.3 no
C15 C16 C17 . 1_555 1_555 107.2(2) no
C15 C16 H16 . 1_555 1_555 126.4 no
C17 C16 H16 . 1_555 1_555 126.4 no
N9 C17 C16 . 1_555 1_555 109.9(2) no
N9 C17 C18 . 1_555 1_555 126.2(2) no
C16 C17 C18 . 1_555 1_555 123.8(2) no
C17 C18 C19 . 1_555 1_555 123.0(2) no
C17 C18 C28 . 1_555 1_555 118.4(2) no
C19 C18 C28 . 1_555 1_555 118.5(2) no
N8 C19 C18 2_555 . 1_555 126.0(2) no
N8 C19 C20 2_555 . 1_555 110.1(2) no
C18 C19 C20 . 1_555 1_555 123.9(3) no
C19 C20 C21 . 1_555 1_555 107.4(3) no
C19 C20 H20 . 1_555 1_555 126.3 no
C21 C20 H20 . 1_555 1_555 126.3 no
C12 C21 C20 2_555 . 1_555 106.9(2) no
C12 C21 H21 2_555 . 1_555 133.1 no
C20 C21 H21 . 1_555 1_555 120.0 no
C13 C22 C23 . 1_555 1_555 121.9(2) no
C13 C22 C27 . 1_555 1_555 119.9(2) no
C23 C22 C27 . 1_555 1_555 118.2(2) no
C22 C23 C24 . 1_555 1_555 121.1(3) no
C22 C23 H23 . 1_555 1_555 119.5 no
C24 C23 H23 . 1_555 1_555 119.4 no
C23 C24 C25 . 1_555 1_555 119.4(3) no
C23 C24 H24 . 1_555 1_555 120.2 no
C25 C24 H24 . 1_555 1_555 120.4 no
C24 C25 C26 . 1_555 1_555 120.9(3) no
C24 C25 H25 . 1_555 1_555 119.5 no
C26 C25 H25 . 1_555 1_555 119.6 no
C25 C26 C27 . 1_555 1_555 120.2(3) no
C25 C26 H26 . 1_555 1_555 120.0 no
C27 C26 H26 . 1_555 1_555 119.9 no
C22 C27 C26 . 1_555 1_555 120.2(3) no
C22 C27 H27 . 1_555 1_555 119.9 no
C26 C27 H27 . 1_555 1_555 119.9 no
C18 C28 C29 . 1_555 1_555 120.5(2) no
C18 C28 C33 . 1_555 1_555 121.1(2) no
C29 C28 C33 . 1_555 1_555 118.4(3) no
C28 C29 C30 . 1_555 1_555 120.2(3) no
C28 C29 H29 . 1_555 1_555 119.9 no
C30 C29 H29 . 1_555 1_555 119.9 no
C29 C30 C31 . 1_555 1_555 120.5(3) no
C29 C30 H30 . 1_555 1_555 119.8 no
C31 C30 H30 . 1_555 1_555 119.7 no
C30 C31 C32 . 1_555 1_555 119.7(3) no
C30 C31 H31 . 1_555 1_555 120.2 no
C32 C31 H31 . 1_555 1_555 120.1 no
C31 C32 C33 . 1_555 1_555 120.7(3) no
C31 C32 H32 . 1_555 1_555 119.6 no
C33 C32 H32 . 1_555 1_555 119.7 no
C28 C33 C32 . 1_555 1_555 120.5(2) no
C28 C33 H33 . 1_555 1_555 119.8 no
C32 C33 H33 . 1_555 1_555 119.7 no
O5 C34 N10 . 1_555 1_555 125.3(7) no
O5 C34 H34 . 1_555 1_555 116.4 no
N10 C34 H34 . 1_555 1_555 118.3 no
N10 C35 H35A . 1_555 1_555 109.1 no
N10 C35 H35B . 1_555 1_555 109.6 no
N10 C35 H35C . 1_555 1_555 109.2 no
H35A C35 H35B . 1_555 1_555 109.9 no
H35A C35 H35C . 1_555 1_555 109.3 no
H35B C35 H35C . 1_555 1_555 109.7 no
N10 C36 H36A . 1_555 1_555 109.9 no
N10 C36 H36B . 1_555 1_555 109.2 no
N10 C36 H36C . 1_555 1_555 109.4 no
H36A C36 H36B . 1_555 1_555 109.3 no
H36A C36 H36C . 1_555 1_555 109.8 no
H36B C36 H36C . 1_555 1_555 109.2 no
O6 C37 N11 . 1_555 1_555 123.5(8) no
O6 C37 H37 . 1_555 1_555 118.3 no
N11 C37 H37 . 1_555 1_555 118.2 no
N11 C38 H38A . 1_555 1_555 109.4 no
N11 C38 H38B . 1_555 1_555 109.4 no
N11 C38 H38C . 1_555 1_555 109.2 no
H38A C38 H38B . 1_555 1_555 109.6 no
H38A C38 H38C . 1_555 1_555 109.7 no
H38B C38 H38C . 1_555 1_555 109.6 no
N11 C39 H39A . 1_555 1_555 110.4 no
N11 C39 H39B . 1_555 1_555 109.8 no
N11 C39 H39C . 1_555 1_555 109.9 no
H39A C39 H39B . 1_555 1_555 109.1 no
H39A C39 H39C . 1_555 1_555 109.1 no
H39B C39 H39C . 1_555 1_555 108.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O4 . . 1.962(2) yes
Co1 O4 . 2_555 1.962(2) no
Co1 N7 . . 1.962(2) yes
Co1 N7 . 2_555 1.962(2) no
Co1 N8 . . 1.983(2) yes
Co1 N8 . 2_555 1.983(2) no
Co1 N9 . . 1.981(2) yes
Co1 N9 . 2_555 1.981(2) no
O5 C34 . . 1.270(10) no
O6 C37 . . 1.247(9) no
N7 O2 . . 1.214(4) yes
N7 O3 . . 1.255(6) yes
N8 C12 . . 1.375(3) no
N8 C19 . 2_555 1.380(4) no
N9 C14 . . 1.377(3) no
N9 C17 . . 1.382(3) no
N10 C34 . . 1.300(10) no
N10 C35 . . 1.42(2) no
N10 C36 . . 1.440(10) no
N11 C37 . . 1.300(10) no
N11 C38 . . 1.451(10) no
N11 C39 . . 1.43(2) no
C12 C13 . . 1.387(4) no
C12 C21 . 2_555 1.438(4) no
C13 C14 . . 1.390(4) no
C13 C22 . . 1.489(3) no
C14 C15 . . 1.437(4) no
C15 C16 . . 1.339(4) no
C15 H15 . . .950 no
C16 C17 . . 1.438(3) no
C16 H16 . . .950 no
C17 C18 . . 1.380(3) no
C18 C19 . . 1.389(3) no
C18 C28 . . 1.506(4) no
C19 C20 . . 1.434(3) no
C20 C21 . . 1.341(4) no
C20 H20 . . .950 no
C21 H21 . . .950 no
C22 C23 . . 1.385(4) no
C22 C27 . . 1.385(3) no
C23 C24 . . 1.381(4) no
C23 H23 . . .950 no
C24 C25 . . 1.361(5) no
C24 H24 . . .951 no
C25 C26 . . 1.355(5) no
C25 H25 . . .950 no
C26 C27 . . 1.388(4) no
C26 H26 . . .950 no
C27 H27 . . .950 no
C28 C29 . . 1.381(4) no
C28 C33 . . 1.374(4) no
C29 C30 . . 1.390(5) no
C29 H29 . . .950 no
C30 C31 . . 1.362(5) no
C30 H30 . . .950 no
C31 C32 . . 1.349(5) no
C31 H31 . . .950 no
C32 C33 . . 1.390(5) no
C32 H32 . . .950 no
C33 H33 . . .950 no
C34 H34 . . .947 no
C35 H35A . . .950 no
C35 H35B . . .946 no
C35 H35C . . .952 no
C36 H36A . . .947 no
C36 H36B . . .955 no
C36 H36C . . .949 no
C37 H37 . . .947 no
C38 H38A . . .948 no
C38 H38B . . .950 no
C38 H38C . . .949 no
C39 H39A . . .948 no
C39 H39B . . .956 no
C39 H39C . . .956 no
