#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321961.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_4321961
loop_
_publ_author_name
'David M. L. Goodgame'
'David A. Grachvogel'
'Izhar Hussain'
'Andrew J. P. White'
'David J. Williams'
_publ_section_title
;
 Formation of Polymeric Network Arrays by Complexes of Manganese(II) or
 Cobalt(II) with Alkane Chain Linked Bis(amide) Ligands of Biological
 Relevance
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2057
_journal_page_last               2063
_journal_paper_doi               10.1021/ic9812609
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C17 H36 Br2 Mn N3 O4'
_chemical_formula_weight         561.25
_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   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.334(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.404(3)
_cell_length_b                   11.262(2)
_cell_length_c                   21.160(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.66
_cell_volume                     5681.3(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.1396
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5037
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        39.98
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.299
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.209
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3733
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.200
_refine_ls_R_factor_all          0.2159
_refine_ls_R_factor_obs          0.0857
_refine_ls_shift/esd_max         0.257
_refine_ls_shift/esd_mean        0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3250
_refine_ls_wR_factor_obs         0.2235
_reflns_number_observed          1889
_reflns_number_total             4913
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9812609_2.cif
_cod_data_source_block           DMLG9713
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5681.3(12)
_cod_database_code               4321961
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn -0.5000 1.3214(2) -0.2500 0.0680(6) Uani 1 d S .
Br1 Br -0.45959(6) 1.19842(15) -0.15401(8) 0.1183(5) Uani 1 d . .
Br2 Br -0.57577(5) 1.44784(12) -0.22303(6) 0.0877(3) Uani 1 d . .
Mn2 Mn -0.2500 0.7500 0.0000 0.0602(5) Uani 1 d S .
C1 C -0.3137(4) 0.5980(10) 0.1163(5) 0.080(3) Uani 1 d . .
H1A H -0.3372(4) 0.5639(10) 0.1427(5) 0.119 Uiso 1 calc R .
H1B H -0.2760(4) 0.6045(10) 0.1411(5) 0.119 Uiso 1 calc R .
H1C H -0.3142(4) 0.5481(10) 0.0794(5) 0.119 Uiso 1 calc R .
O2 O -0.3116(3) 0.7786(6) 0.0597(3) 0.069(2) Uani 1 d . .
C2 C -0.3345(4) 0.7145(9) 0.0949(4) 0.067(3) Uani 1 d . .
N3 N -0.3790(3) 0.7546(8) 0.1149(4) 0.075(2) Uani 1 d . .
H3A H -0.3947(3) 0.7081(8) 0.1380(4) 0.090 Uiso 1 calc R .
C4 C -0.4026(5) 0.8705(10) 0.1005(5) 0.082(3) Uani 1 d . .
H4A H -0.3729(5) 0.9250(10) 0.0960(5) 0.098 Uiso 1 calc R .
H4B H -0.4182(5) 0.8974(10) 0.1365(5) 0.098 Uiso 1 calc R .
C5 C -0.4485(4) 0.8744(11) 0.0387(5) 0.083(3) Uani 1 d . .
H5A H -0.4769(4) 0.8156(11) 0.0415(5) 0.100 Uiso 1 calc R .
H5B H -0.4323(4) 0.8545(11) 0.0019(5) 0.100 Uiso 1 calc R .
C6 C -0.4760(5) 0.9977(12) 0.0280(5) 0.091(4) Uani 1 d . .
H6A H -0.4889(5) 1.0205(12) 0.0666(5) 0.109 Uiso 1 calc R .
H6B H -0.4481(5) 1.0551(12) 0.0216(5) 0.109 Uiso 1 calc R .
C7 C -0.3243(7) 1.0413(15) -0.0374(7) 0.140(6) Uani 1 d . .
H7A H -0.3540(7) 1.0979(15) -0.0500(7) 0.210 Uiso 1 calc R .
H7B H -0.2895(7) 1.0758(15) -0.0425(7) 0.210 Uiso 1 calc R .
H7C H -0.3214(7) 1.0194(15) 0.0070(7) 0.210 Uiso 1 calc R .
O8 O -0.3062(3) 0.8465(7) -0.0745(3) 0.085(2) Uani 1 d . .
C8 C -0.3363(4) 0.9350(13) -0.0785(5) 0.092(4) Uani 1 d D .
N9 N -0.3845(5) 0.9327(9) -0.1244(5) 0.172(6) Uani 1 d DU .
H9A H -0.4071(5) 0.9921(9) -0.1285(5) 0.207 Uiso 1 calc R .
C10 C -0.3983(4) 0.8303(12) -0.1670(9) 0.298(11) Uani 1 d DU .
H10A H -0.3893(4) 0.7558(12) -0.1441(9) 0.358 Uiso 1 calc R .
H10B H -0.3803(4) 0.8337(12) -0.2036(9) 0.358 Uiso 1 calc R .
C11 C -0.4608(4) 0.8505(13) -0.1868(7) 0.328(10) Uani 1 d DU .
H11A H -0.4808(4) 0.8230(13) -0.1546(7) 0.393 Uiso 1 calc R .
H11B H -0.4704(4) 0.9324(13) -0.1982(7) 0.393 Uiso 1 calc R .
C12 C -0.4684(2) 0.7703(18) -0.2447(9) 0.339(12) Uani 1 d DU .
H12A H -0.4521(2) 0.6922(18) -0.2346(9) 0.407 Uiso 1 calc R .
H12B H -0.4549(2) 0.8051(18) -0.2805(9) 0.407 Uiso 1 calc R .
C13 C -0.2946(5) 0.5846(13) -0.1519(6) 0.105(4) Uani 1 d . .
H13A H -0.3172(5) 0.5479(13) -0.1895(6) 0.157 Uiso 1 calc R .
H13B H -0.2570(5) 0.5545(13) -0.1449(6) 0.157 Uiso 1 calc R .
H13C H -0.2942(5) 0.6690(13) -0.1581(6) 0.157 Uiso 1 calc R .
O14 O -0.2966(3) 0.5959(6) -0.0395(3) 0.079(2) Uani 1 d . .
C14 C -0.3189(4) 0.5573(11) -0.0939(5) 0.082(3) Uani 1 d . .
N15 N -0.3634(4) 0.4878(13) -0.1020(5) 0.121(4) Uani 1 d . .
H15A H -0.3772(4) 0.4627(13) -0.1405(5) 0.145 Uiso 1 calc R .
C16 C -0.3907(6) 0.4506(16) -0.0507(7) 0.133(6) Uani 1 d . .
H16A H -0.3650(6) 0.4612(16) -0.0093(7) 0.159 Uiso 1 calc R .
H16B H -0.3997(6) 0.3668(16) -0.0558(7) 0.159 Uiso 1 calc R .
C17 C -0.4429(6) 0.5183(15) -0.0507(7) 0.118(5) Uani 1 d . .
H17A H -0.4680(6) 0.5109(15) -0.0928(7) 0.142 Uiso 1 calc R .
H17B H -0.4338(6) 0.6017(15) -0.0433(7) 0.142 Uiso 1 calc R .
C18 C -0.4725(5) 0.4732(13) 0.0016(6) 0.111(4) Uani 1 d . .
H18A H -0.4769(5) 0.3877(13) -0.0026(6) 0.133 Uiso 1 calc R .
H18B H -0.4489(5) 0.4895(13) 0.0438(6) 0.133 Uiso 1 calc R .
O50 O -0.2732(7) 0.2860(12) 0.1630(10) 0.283(10) Uani 1 d D .
C51 C -0.2276(10) 0.2617(18) 0.1939(14) 0.237(16) Uani 0.489(12) d PD 1
H51A H -0.2075(10) 0.2199(18) 0.1658(14) 0.285 Uiso 0.489(12) calc PR 1
H51B H -0.2322(10) 0.2069(18) 0.2277(14) 0.285 Uiso 0.489(12) calc PR 1
C52 C -0.1923(10) 0.3603(22) 0.2242(11) 0.112(10) Uani 0.489(12) d PD 1
H52A H -0.1566(10) 0.3301(22) 0.2464(11) 0.169 Uiso 0.489(12) calc PR 1
H52B H -0.2102(10) 0.3997(22) 0.2545(11) 0.169 Uiso 0.489(12) calc PR 1
H52C H -0.1870(10) 0.4156(22) 0.1915(11) 0.169 Uiso 0.489(12) calc PR 1
C53 C -0.3590(10) 0.2526(23) 0.1294(13) 0.131(12) Uani 0.511(12) d PD 2
H53A H -0.3872(10) 0.1931(23) 0.1292(13) 0.196 Uiso 0.511(12) calc PR 2
H53B H -0.3556(10) 0.2684(23) 0.0858(13) 0.196 Uiso 0.511(12) calc PR 2
H53C H -0.3694(10) 0.3241(23) 0.1484(13) 0.196 Uiso 0.511(12) calc PR 2
C54 C -0.3044(9) 0.2096(22) 0.1675(18) 0.191(15) Uani 0.511(12) d PD 2
H54A H -0.3062(9) 0.1968(22) 0.2123(18) 0.229 Uiso 0.511(12) calc PR 2
H54B H -0.2934(9) 0.1362(22) 0.1498(18) 0.229 Uiso 0.511(12) calc PR 2
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'
Br Br -0.2901 2.4595 '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
Br1 Mn1 Br1 112.16(12) 2_454 . ?
Br1 Mn1 Br2 108.40(5) 2_454 2_454 ?
Br1 Mn1 Br2 108.75(5) . 2_454 ?
Br1 Mn1 Br2 108.75(5) 2_454 . ?
Br1 Mn1 Br2 108.40(5) . . ?
Br2 Mn1 Br2 110.38(11) 2_454 . ?
O14 Mn2 O14 180.0 . 7_465 ?
O14 Mn2 O8 85.5(3) . . ?
O14 Mn2 O8 94.5(3) 7_465 . ?
O14 Mn2 O8 94.5(3) . 7_465 ?
O14 Mn2 O8 85.5(3) 7_465 7_465 ?
O8 Mn2 O8 180.0 . 7_465 ?
O14 Mn2 O2 88.3(3) . . ?
O14 Mn2 O2 91.7(3) 7_465 . ?
O8 Mn2 O2 86.5(3) . . ?
O8 Mn2 O2 93.5(3) 7_465 . ?
O14 Mn2 O2 91.7(3) . 7_465 ?
O14 Mn2 O2 88.3(3) 7_465 7_465 ?
O8 Mn2 O2 93.5(3) . 7_465 ?
O8 Mn2 O2 86.5(3) 7_465 7_465 ?
O2 Mn2 O2 180.0 . 7_465 ?
C2 O2 Mn2 135.2(7) . . ?
O2 C2 N3 119.6(9) . . ?
O2 C2 C1 122.7(9) . . ?
N3 C2 C1 117.7(9) . . ?
C2 N3 C4 124.1(9) . . ?
N3 C4 C5 113.3(9) . . ?
C4 C5 C6 111.7(9) . . ?
C6 C6 C5 113.3(13) 5_475 . ?
C8 O8 Mn2 137.5(7) . . ?
O8 C8 N9 116.5(12) . . ?
O8 C8 C7 125.3(10) . . ?
N9 C8 C7 118.2(11) . . ?
C8 N9 C10 120.6(11) . . ?
N9 C10 C11 98.0(9) . . ?
C12 C11 C10 94.4(9) . . ?
C11 C12 C12 93.7(12) . 2_454 ?
C14 O14 Mn2 137.3(8) . . ?
O14 C14 N15 120.8(11) . . ?
O14 C14 C13 120.9(10) . . ?
N15 C14 C13 118.2(10) . . ?
C14 N15 C16 124.9(11) . . ?
N15 C16 C17 112.5(14) . . ?
C16 C17 C18 111.5(13) . . ?
C18 C18 C17 113.6(15) 5_465 . ?
O50 C51 C52 117.2(19) . . ?
O50 C54 C53 103.9(22) . . ?
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 Br1 2.482(2) 2_454 ?
Mn1 Br1 2.482(2) . ?
Mn1 Br2 2.495(2) 2_454 ?
Mn1 Br2 2.495(2) . ?
Mn2 O14 2.145(7) . ?
Mn2 O14 2.145(7) 7_465 ?
Mn2 O8 2.151(7) . ?
Mn2 O8 2.151(7) 7_465 ?
Mn2 O2 2.185(6) . ?
Mn2 O2 2.185(6) 7_465 ?
C1 C2 1.444(14) . ?
O2 C2 1.251(12) . ?
C2 N3 1.328(13) . ?
N3 C4 1.432(14) . ?
C4 C5 1.530(14) . ?
C5 C6 1.54(2) . ?
C6 C6 1.48(2) 5_475 ?
C7 C8 1.47(2) . ?
O8 C8 1.230(14) . ?
C8 N9 1.357(13) . ?
N9 C10 1.457(9) . ?
C10 C11 1.509(9) . ?
C11 C12 1.502(10) . ?
C12 C12 1.512(7) 2_454 ?
C13 C14 1.50(2) . ?
O14 C14 1.243(12) . ?
C14 N15 1.32(2) . ?
N15 C16 1.45(2) . ?
C16 C17 1.48(2) . ?
C17 C18 1.53(2) . ?
C18 C18 1.46(3) 5_465 ?
O50 C54 1.17(2) . ?
O50 C51 1.20(2) . ?
C51 C52 1.47(2) . ?
C53 C54 1.48(2) . ?
