#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:54:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180362 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/31/7203107.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_7203107
loop_
_publ_author_name
'Karmakar, Tapan K.'
'Aromí, Guillem'
'Ghosh, Barindra K.'
'Usman, A.'
'Fun, Hoong-Kun'
'Mallah, Talal'
'Behrens, U.'
'Solans, Xavier'
'Chandra, Swapan K.'
_publ_section_title
;
 Unexpected diversity and novel features within a family of new
 azide-bridged MnII complexes of pyridyl/imine ligands
;
_journal_issue                   3
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              278
_journal_paper_doi               10.1039/b510701f
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C16 H18 Cl Mn N7 O4'
_chemical_formula_weight         462.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5606(6)
_cell_length_b                   17.2500(8)
_cell_length_c                   18.1617(9)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    153(2)
_cell_volume                     3935.1(3)
_computing_cell_refinement       'SMART (Bruker axs)'
_computing_data_collection       'SMART (Bruker axs)'
_computing_data_reduction        'SAINT (Bruker axs)'
_computing_molecular_graphics    'SHELXTL V5.10 NT (Sheldrick, 1998)'
_computing_publication_material  'SHELXTL V5.10 NT (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44314
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.9202
_exptl_absorpt_correction_T_min  0.7284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker axs)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0998P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                3109
_reflns_number_total             4509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b510701f.txt
_cod_data_source_block           T-Mn65a
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7203107
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
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 0.73528(4) 0.7500 0.02072(19) Uani 1 2 d S . .
Mn2 Mn 0.5000 0.53408(4) 0.7500 0.02223(19) Uani 1 2 d S . .
N1 N 0.5542(2) 0.63350(14) 0.68228(13) 0.0240(6) Uani 1 1 d . . .
N2 N 0.5461(2) 0.63369(16) 0.61589(16) 0.0317(7) Uani 1 1 d . . .
N3 N 0.5388(3) 0.6351(2) 0.55313(16) 0.0491(9) Uani 1 1 d . . .
N4 N 0.4666(2) 0.80555(17) 0.85378(16) 0.0338(7) Uani 1 1 d . . .
N5 N 0.5414(2) 0.44453(19) 0.66500(18) 0.0402(8) Uani 1 1 d . . .
N6 N 0.6578(2) 0.75309(15) 0.80539(14) 0.0247(6) Uani 1 1 d . . .
N7 N 0.3500(2) 0.51443(15) 0.68381(14) 0.0251(6) Uani 1 1 d . . .
C1 C 0.5441(3) 0.8038(2) 0.8993(2) 0.0376(9) Uani 1 1 d . . .
H1 H 0.5332 0.8196 0.9488 0.045 Uiso 1 1 calc R . .
C2 C 0.6493(3) 0.7776(2) 0.87586(19) 0.0322(8) Uani 1 1 d . . .
C3 C 0.7357(3) 0.7774(2) 0.9240(2) 0.0417(9) Uani 1 1 d . . .
H3 H 0.7268 0.7919 0.9741 0.050 Uiso 1 1 calc R . .
C4 C 0.8338(3) 0.7558(2) 0.8978(2) 0.0411(9) Uani 1 1 d . . .
H4 H 0.8942 0.7570 0.9292 0.049 Uiso 1 1 calc R . .
C5 C 0.8439(3) 0.7323(2) 0.8253(2) 0.0334(8) Uani 1 1 d . . .
H5 H 0.9111 0.7175 0.8059 0.040 Uiso 1 1 calc R . .
C6 C 0.7534(3) 0.73099(19) 0.78185(18) 0.0297(7) Uani 1 1 d . . .
H6 H 0.7599 0.7133 0.7325 0.036 Uiso 1 1 calc R . .
C7 C 0.3627(3) 0.8334(2) 0.8809(2) 0.0418(9) Uani 1 1 d . . .
H7A H 0.3642 0.8387 0.9351 0.050 Uiso 1 1 calc R . .
H7B H 0.3059 0.7961 0.8676 0.050 Uiso 1 1 calc R . .
C8 C 0.3414(3) 0.9107(2) 0.8456(2) 0.0490(10) Uani 1 1 d . . .
H8A H 0.3456 0.9051 0.7915 0.059 Uiso 1 1 calc R . .
H8B H 0.3972 0.9478 0.8611 0.059 Uiso 1 1 calc R . .
C9 C 0.2292(3) 0.9446(2) 0.8667(2) 0.0489(10) Uani 1 1 d . . .
H9A H 0.2228 0.9470 0.9210 0.059 Uiso 1 1 calc R . .
H9B H 0.2229 0.9980 0.8473 0.059 Uiso 1 1 calc R . .
C10 C 0.1415(3) 0.8964(2) 0.8365(2) 0.0467(10) Uani 1 1 d . . .
H10A H 0.1308 0.8500 0.8677 0.056 Uiso 1 1 calc R . .
H10B H 0.1596 0.8790 0.7861 0.056 Uiso 1 1 calc R . .
C11 C 0.4703(3) 0.4350(3) 0.6153(2) 0.0459(10) Uani 1 1 d . . .
H11 H 0.4845 0.4021 0.5745 0.055 Uiso 1 1 calc R . .
C12 C 0.3663(3) 0.4747(2) 0.62068(19) 0.0343(8) Uani 1 1 d . . .
C13 C 0.2883(3) 0.4667(2) 0.5683(2) 0.0445(10) Uani 1 1 d . . .
H13 H 0.3025 0.4397 0.5238 0.053 Uiso 1 1 calc R . .
C14 C 0.1889(3) 0.4985(2) 0.5811(2) 0.0477(10) Uani 1 1 d . . .
H14 H 0.1342 0.4946 0.5452 0.057 Uiso 1 1 calc R . .
C15 C 0.1703(3) 0.5361(2) 0.6472(2) 0.0440(10) Uani 1 1 d . . .
H15 H 0.1020 0.5564 0.6587 0.053 Uiso 1 1 calc R . .
C16 C 0.2542(3) 0.54332(19) 0.6962(2) 0.0335(8) Uani 1 1 d . . .
H16 H 0.2422 0.5704 0.7410 0.040 Uiso 1 1 calc R . .
Cl2 Cl 0.89134(6) 0.63819(5) 0.60732(4) 0.0280(2) Uani 1 1 d . . .
O1 O 0.9194(2) 0.61973(17) 0.68149(13) 0.0476(7) Uani 1 1 d . . .
O2 O 0.9479(3) 0.5900(2) 0.55809(14) 0.0618(9) Uani 1 1 d . . .
O3 O 0.7796(2) 0.63017(18) 0.59589(19) 0.0629(9) Uani 1 1 d . . .
O4 O 0.9177(3) 0.71738(17) 0.59194(19) 0.0672(9) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
N6 Mn1 N6 164.26(14) . 3_656 ?
N6 Mn1 N1 94.85(9) . . ?
N6 Mn1 N1 97.42(10) 3_656 . ?
N6 Mn1 N1 97.42(10) . 3_656 ?
N6 Mn1 N1 94.85(9) 3_656 3_656 ?
N1 Mn1 N1 77.37(13) . 3_656 ?
N6 Mn1 N4 73.69(10) . . ?
N6 Mn1 N4 97.77(10) 3_656 . ?
N1 Mn1 N4 157.34(10) . . ?
N1 Mn1 N4 84.68(10) 3_656 . ?
N6 Mn1 N4 97.77(10) . 3_656 ?
N6 Mn1 N4 73.69(10) 3_656 3_656 ?
N1 Mn1 N4 84.68(10) . 3_656 ?
N1 Mn1 N4 157.34(10) 3_656 3_656 ?
N4 Mn1 N4 115.76(16) . 3_656 ?
N1 Mn2 N1 78.69(13) . 3_656 ?
N1 Mn2 N5 94.57(11) . . ?
N1 Mn2 N5 169.96(11) 3_656 . ?
N1 Mn2 N5 169.96(11) . 3_656 ?
N1 Mn2 N5 94.57(11) 3_656 3_656 ?
N5 Mn2 N5 93.03(18) . 3_656 ?
N1 Mn2 N7 94.41(10) . . ?
N1 Mn2 N7 98.93(9) 3_656 . ?
N5 Mn2 N7 73.98(10) . . ?
N5 Mn2 N7 93.98(10) 3_656 . ?
N1 Mn2 N7 98.93(10) . 3_656 ?
N1 Mn2 N7 94.41(10) 3_656 3_656 ?
N5 Mn2 N7 93.98(10) . 3_656 ?
N5 Mn2 N7 73.98(10) 3_656 3_656 ?
N7 Mn2 N7 162.75(14) . 3_656 ?
N2 N1 Mn2 121.9(2) . . ?
N2 N1 Mn1 121.2(2) . . ?
Mn2 N1 Mn1 101.97(10) . . ?
N3 N2 N1 178.9(4) . . ?
C1 N4 C7 117.8(3) . . ?
C1 N4 Mn1 112.4(2) . . ?
C7 N4 Mn1 127.7(2) . . ?
C11 N5 C10 119.9(3) . 6_657 ?
C11 N5 Mn2 114.3(2) . . ?
C10 N5 Mn2 125.8(2) 6_657 . ?
C6 N6 C2 117.7(3) . . ?
C6 N6 Mn1 127.9(2) . . ?
C2 N6 Mn1 113.4(2) . . ?
C16 N7 C12 118.2(3) . . ?
C16 N7 Mn2 127.7(2) . . ?
C12 N7 Mn2 113.7(2) . . ?
N4 C1 C2 120.6(3) . . ?
N6 C2 C3 122.1(3) . . ?
N6 C2 C1 116.4(3) . . ?
C3 C2 C1 121.6(3) . . ?
C4 C3 C2 118.9(3) . . ?
C3 C4 C5 119.4(3) . . ?
C6 C5 C4 118.2(3) . . ?
N6 C6 C5 123.6(3) . . ?
N4 C7 C8 107.7(3) . . ?
C7 C8 C9 112.7(3) . . ?
C10 C9 C8 111.6(3) . . ?
C9 C10 N5 108.5(3) . 6_567 ?
N5 C11 C12 120.7(3) . . ?
N7 C12 C13 122.1(3) . . ?
N7 C12 C11 115.1(3) . . ?
C13 C12 C11 122.6(3) . . ?
C12 C13 C14 119.2(3) . . ?
C13 C14 C15 118.9(3) . . ?
C16 C15 C14 118.1(3) . . ?
N7 C16 C15 123.3(3) . . ?
O2 Cl2 O3 110.3(2) . . ?
O2 Cl2 O1 109.96(17) . . ?
O3 Cl2 O1 111.01(18) . . ?
O2 Cl2 O4 108.7(2) . . ?
O3 Cl2 O4 106.97(19) . . ?
O1 Cl2 O4 109.83(19) . . ?
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 N6 2.244(2) . ?
Mn1 N6 2.244(2) 3_656 ?
Mn1 N1 2.249(3) . ?
Mn1 N1 2.249(3) 3_656 ?
Mn1 N4 2.280(3) . ?
Mn1 N4 2.280(3) 3_656 ?
Mn2 N1 2.217(3) . ?
Mn2 N1 2.217(3) 3_656 ?
Mn2 N5 2.245(3) . ?
Mn2 N5 2.245(3) 3_656 ?
Mn2 N7 2.260(2) . ?
Mn2 N7 2.260(2) 3_656 ?
N1 N2 1.210(4) . ?
N2 N3 1.144(4) . ?
N4 C1 1.277(4) . ?
N4 C7 1.475(4) . ?
N5 C11 1.281(5) . ?
N5 C10 1.507(5) 6_657 ?
N6 C6 1.330(4) . ?
N6 C2 1.352(4) . ?
N7 C16 1.323(4) . ?
N7 C12 1.351(4) . ?
C1 C2 1.459(5) . ?
C2 C3 1.393(5) . ?
C3 C4 1.371(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.383(4) . ?
C7 C8 1.504(6) . ?
C8 C9 1.572(5) . ?
C9 C10 1.484(5) . ?
C10 N5 1.507(5) 6_567 ?
C11 C12 1.478(5) . ?
C12 C13 1.372(5) . ?
C13 C14 1.384(6) . ?
C14 C15 1.384(5) . ?
C15 C16 1.384(5) . ?
Cl2 O2 1.413(3) . ?
Cl2 O3 1.426(3) . ?
Cl2 O1 1.428(2) . ?
Cl2 O4 1.433(3) . ?
