#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/36/7013646.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_7013646
loop_
_publ_author_name
'Stuart D. Reid'
'Alexander J. Blake'
'Walter Köckenberger'
'Claire Wilson'
'Jason B. Love'
_publ_section_title
;
 Double-stranded, [4 + 4] helicates of Fe(II) and Mn(II) supported by
 an extended dipyrrolide ligand
;
_journal_issue                   23
_journal_name_full               'Dalton Trans.'
_journal_page_first              4387
_journal_page_last               4388
_journal_paper_doi               10.1039/b311093a
_journal_year                    2003
_chemical_formula_moiety         'C42 H62 Mn N8, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H78 Mn N8 O2'
_chemical_formula_weight         878.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.152(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.635(2)
_cell_length_b                   14.208(2)
_cell_length_c                   21.382(2)
_cell_measurement_reflns_used    5104
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.3
_cell_volume                     5029.5(10)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17490
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS version 2.03; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sphenoid
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.30
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0499
_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)+(0.071P)²+4.88P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.126
_refine_ls_wR_factor_ref         0.134
_reflns_number_gt                4797
_reflns_number_total             5926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311093a.txt
_cod_data_source_block           MNPYBU
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        5030(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7013646
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Mn1 Mn 0.5000 0.46757(3) 0.2500 0.02547(12) Uani 1 2 d S . .
N1 N 0.41595(9) 0.33802(11) 0.18281(7) 0.0300(3) Uani 1 1 d . . .
N2 N 0.39342(9) 0.45764(10) 0.27588(7) 0.0269(3) Uani 1 1 d . . .
N3 N 0.54508(9) 0.56032(11) 0.34781(7) 0.0294(3) Uani 1 1 d . . .
N4 N 0.76611(10) 0.54949(13) 0.41288(8) 0.0408(4) Uani 1 1 d . . .
H4A H 0.7752 0.5682 0.4531 0.049 Uiso 1 1 calc R . .
C1 C 0.33948(15) 0.2596(3) 0.07524(13) 0.0706(9) Uani 1 1 d . . .
H1A H 0.3154 0.3187 0.0571 0.106 Uiso 1 1 calc R . .
H1B H 0.3054 0.2278 0.0951 0.106 Uiso 1 1 calc R . .
H1C H 0.3456 0.2213 0.0403 0.106 Uiso 1 1 calc R . .
C2 C 0.46304(18) 0.18485(17) 0.15851(14) 0.0594(7) Uani 1 1 d . . .
H2A H 0.4299 0.1523 0.1790 0.089 Uiso 1 1 calc R . .
H2B H 0.5147 0.1984 0.1915 0.089 Uiso 1 1 calc R . .
H2C H 0.4703 0.1460 0.1243 0.089 Uiso 1 1 calc R . .
C3 C 0.47500(13) 0.32762(15) 0.09564(10) 0.0399(5) Uani 1 1 d . . .
H3A H 0.4496 0.3855 0.0762 0.060 Uiso 1 1 calc R . .
H3B H 0.4823 0.2884 0.0616 0.060 Uiso 1 1 calc R . .
H3C H 0.5266 0.3409 0.1288 0.060 Uiso 1 1 calc R . .
C4 C 0.42187(12) 0.27698(15) 0.12786(10) 0.0374(4) Uani 1 1 d . . .
C5 C 0.36242(11) 0.31738(14) 0.20855(9) 0.0330(4) Uani 1 1 d . . .
H5A H 0.3307 0.2640 0.1940 0.040 Uiso 1 1 calc R . .
C6 C 0.35052(11) 0.37520(14) 0.25944(9) 0.0314(4) Uani 1 1 d . . .
C7 C 0.30101(12) 0.36401(16) 0.29733(10) 0.0393(5) Uani 1 1 d . . .
H7A H 0.2660 0.3142 0.2953 0.047 Uiso 1 1 calc R . .
C8 C 0.31443(12) 0.44273(15) 0.33917(10) 0.0377(4) Uani 1 1 d . . .
H8A H 0.2904 0.4553 0.3707 0.045 Uiso 1 1 calc R . .
C9 C 0.37106(10) 0.49860(14) 0.32421(8) 0.0293(4) Uani 1 1 d . . .
C10 C 0.40695(11) 0.59248(13) 0.35204(9) 0.0308(4) Uani 1 1 d . . .
C11 C 0.37079(12) 0.62686(16) 0.40379(10) 0.0414(5) Uani 1 1 d . . .
H11A H 0.3820 0.5817 0.4392 0.062 Uiso 1 1 calc R . .
H11B H 0.3134 0.6340 0.3830 0.062 Uiso 1 1 calc R . .
H11C H 0.3944 0.6863 0.4215 0.062 Uiso 1 1 calc R . .
C12 C 0.38809(12) 0.66594(14) 0.29557(10) 0.0377(4) Uani 1 1 d . . .
H12A H 0.4103 0.6453 0.2627 0.057 Uiso 1 1 calc R . .
H12B H 0.4116 0.7253 0.3136 0.057 Uiso 1 1 calc R . .
H12C H 0.3306 0.6729 0.2752 0.057 Uiso 1 1 calc R . .
C13 C 0.49835(11) 0.58236(13) 0.38339(8) 0.0289(4) Uani 1 1 d . . .
C14 C 0.54442(12) 0.59407(14) 0.45206(9) 0.0351(4) Uani 1 1 d . . .
H14A H 0.5246 0.6084 0.4860 0.042 Uiso 1 1 calc R . .
C15 C 0.62347(12) 0.58030(14) 0.45863(9) 0.0358(4) Uani 1 1 d . . .
H15A H 0.6679 0.5837 0.4977 0.043 Uiso 1 1 calc R . .
C16 C 0.62422(11) 0.55968(14) 0.39384(9) 0.0314(4) Uani 1 1 d . . .
C17 C 0.68971(11) 0.54418(14) 0.37357(10) 0.0343(4) Uani 1 1 d . . .
H17A H 0.6792 0.5289 0.3291 0.041 Uiso 1 1 calc R . .
C18 C 0.83745(12) 0.52634(19) 0.39436(11) 0.0477(5) Uani 1 1 d . . .
C19 C 0.82333(14) 0.5530(2) 0.32240(12) 0.0578(7) Uani 1 1 d . . .
H19A H 0.7792 0.5168 0.2934 0.087 Uiso 1 1 calc R . .
H19B H 0.8713 0.5404 0.3122 0.087 Uiso 1 1 calc R . .
H19C H 0.8106 0.6188 0.3161 0.087 Uiso 1 1 calc R . .
C20 C 0.85362(18) 0.4217(2) 0.40517(19) 0.0774(9) Uani 1 1 d . . .
H20A H 0.8088 0.3871 0.3756 0.116 Uiso 1 1 calc R . .
H20B H 0.8605 0.4060 0.4505 0.116 Uiso 1 1 calc R . .
H20C H 0.9018 0.4058 0.3963 0.116 Uiso 1 1 calc R . .
C21 C 0.90750(15) 0.5837(3) 0.44057(14) 0.0758(10) Uani 1 1 d . . .
H21A H 0.8960 0.6496 0.4328 0.114 Uiso 1 1 calc R . .
H21B H 0.9560 0.5687 0.4319 0.114 Uiso 1 1 calc R . .
H21C H 0.9146 0.5690 0.4861 0.114 Uiso 1 1 calc R . .
O1S O 0.68479(10) 0.90493(12) 0.44131(8) 0.0504(4) Uani 1 1 d . . .
C1S C 0.63147(16) 0.96547(19) 0.39385(13) 0.0562(6) Uani 1 1 d . . .
H1SA H 0.6615 1.0115 0.3783 0.067 Uiso 1 1 calc R . .
H1SB H 0.5967 0.9985 0.4132 0.067 Uiso 1 1 calc R . .
C2S C 0.5838(3) 0.9057(4) 0.3391(2) 0.134(2) Uani 1 1 d . . .
H2SA H 0.5268 0.9204 0.3273 0.161 Uiso 1 1 calc R . .
H2SB H 0.5993 0.9162 0.3003 0.161 Uiso 1 1 calc R . .
C3S C 0.5978(3) 0.8125(3) 0.3596(2) 0.1196(17) Uani 1 1 d . . .
H3SA H 0.6053 0.7743 0.3245 0.143 Uiso 1 1 calc R . .
H3SB H 0.5523 0.7877 0.3700 0.143 Uiso 1 1 calc R . .
C4S C 0.67018(19) 0.8108(2) 0.41827(16) 0.0709(8) Uani 1 1 d . . .
H4SA H 0.6623 0.7707 0.4523 0.085 Uiso 1 1 calc R . .
H4SB H 0.7155 0.7869 0.4072 0.085 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'
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'
Mn Mn 0.3368 0.7283 '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
N2 Mn1 N2 172.44(8) 2_655 . ?
N2 Mn1 N3 102.00(5) 2_655 . ?
N2 Mn1 N3 82.28(5) . . ?
N3 Mn1 N3 112.30(8) . 2_655 ?
N2 Mn1 N1 101.75(5) 2_655 . ?
N2 Mn1 N1 72.46(5) . . ?
N3 Mn1 N1 151.05(5) . . ?
N3 Mn1 N1 87.12(5) 2_655 . ?
N1 Mn1 N1 84.48(7) . 2_655 ?
C5 N1 C4 117.86(16) . . ?
C5 N1 Mn1 107.60(12) . . ?
C4 N1 Mn1 134.07(11) . . ?
C9 N2 C6 106.36(15) . . ?
C9 N2 Mn1 132.87(12) . . ?
C6 N2 Mn1 116.48(11) . . ?
C13 N3 C16 105.16(14) . . ?
C13 N3 Mn1 123.24(12) . . ?
C16 N3 Mn1 124.50(12) . . ?
C17 N4 C18 126.24(18) . . ?
N1 C4 C1 111.64(17) . . ?
N1 C4 C3 107.62(15) . . ?
C1 C4 C3 108.80(19) . . ?
N1 C4 C2 108.14(17) . . ?
C1 C4 C2 111.7(2) . . ?
C3 C4 C2 108.86(18) . . ?
N1 C5 C6 121.13(17) . . ?
N2 C6 C7 110.47(17) . . ?
N2 C6 C5 118.09(15) . . ?
C7 C6 C5 131.44(18) . . ?
C6 C7 C8 106.22(17) . . ?
C9 C8 C7 106.52(17) . . ?
N2 C9 C8 110.43(17) . . ?
N2 C9 C10 119.15(15) . . ?
C8 C9 C10 130.42(16) . . ?
C9 C10 C13 109.06(14) . . ?
C9 C10 C11 110.11(16) . . ?
C13 C10 C11 110.61(15) . . ?
C9 C10 C12 109.97(15) . . ?
C13 C10 C12 108.55(15) . . ?
C11 C10 C12 108.52(16) . . ?
N3 C13 C14 111.72(16) . . ?
N3 C13 C10 122.51(15) . . ?
C14 C13 C10 125.77(16) . . ?
C15 C14 C13 106.81(16) . . ?
C14 C15 C16 106.34(16) . . ?
C17 C16 N3 121.12(16) . . ?
C17 C16 C15 128.87(17) . . ?
N3 C16 C15 109.96(16) . . ?
N4 C17 C16 124.71(18) . . ?
N4 C18 C20 108.03(19) . . ?
N4 C18 C19 110.95(18) . . ?
C20 C18 C19 110.8(2) . . ?
N4 C18 C21 106.3(2) . . ?
C20 C18 C21 111.0(2) . . ?
C19 C18 C21 109.6(2) . . ?
C1S O1S C4S 109.2(2) . . ?
O1S C1S C2S 106.2(3) . . ?
C3S C2S C1S 108.1(3) . . ?
C2S C3S C4S 107.3(3) . . ?
O1S C4S C3S 106.6(3) . . ?
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
Mn1 N2 2.1390(14) . ?
Mn1 N3 2.3659(15) . ?
Mn1 N1 2.4863(15) . ?
N1 C5 1.280(2) . ?
N1 C4 1.493(2) . ?
N2 C9 1.357(2) . ?
N2 C6 1.373(2) . ?
N3 C13 1.337(2) . ?
N3 C16 1.404(2) . ?
N4 C17 1.322(2) . ?
N4 C18 1.480(3) . ?
C1 C4 1.520(3) . ?
C2 C4 1.530(3) . ?
C3 C4 1.521(3) . ?
C5 C6 1.435(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.401(3) . ?
C8 C9 1.396(3) . ?
C9 C10 1.508(3) . ?
C10 C13 1.524(2) . ?
C10 C11 1.535(2) . ?
C10 C12 1.543(3) . ?
C13 C14 1.422(2) . ?
C14 C15 1.366(3) . ?
C15 C16 1.420(3) . ?
C16 C17 1.384(3) . ?
C18 C20 1.516(4) . ?
C18 C19 1.520(3) . ?
C18 C21 1.525(4) . ?
O1S C1S 1.413(3) . ?
O1S C4S 1.418(3) . ?
C1S C2S 1.457(5) . ?
C2S C3S 1.390(6) . ?
C3S C4S 1.449(5) . ?
