#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307875.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_4307875
loop_
_publ_author_name
'Carole Duboc'
'Thida Phoeung'
'Samir Zein'
'Jacques Pécaut'
'Marie-Noëlle Collomb'
'Frank Neese'
_publ_section_title
;
Origin of the Zero-Field Splitting in Mononuclear Octahedral Dihalide
MnII Complexes: An Investigation by Multifrequency High-Field Electron
Paramagnetic Resonance and Density Functional Theory
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4905
_journal_page_last               4916
_journal_paper_doi               10.1021/ic062384l
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C18 H18 I2 Mn N4'
_chemical_formula_weight         599.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1075(18)
_cell_length_b                   16.228(3)
_cell_length_c                   14.137(3)
_cell_measurement_temperature    298(2)
_cell_volume                     2088.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13004
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.597
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0298
_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)+(0.0164P)²+1.8243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                4152
_reflns_number_total             4935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062384l-file005.cif
_cod_data_source_block           struc
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2088.2(7)
_cod_database_code               4307875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Mn Mn 0.51028(5) 0.63530(3) 0.74768(3) 0.03387(10) Uani 1 1 d . . .
I1 I 0.68186(3) 0.605675(14) 0.912199(15) 0.05467(8) Uani 1 1 d . . .
I2 I 0.63862(2) 0.508006(13) 0.635266(14) 0.04182(6) Uani 1 1 d . . .
N1 N 0.3409(3) 0.68192(15) 0.62931(17) 0.0382(6) Uani 1 1 d . . .
N2 N 0.3010(3) 0.56191(15) 0.76501(16) 0.0368(5) Uani 1 1 d . . .
N3 N 0.3876(3) 0.74461(15) 0.81507(18) 0.0420(6) Uani 1 1 d . . .
N4 N 0.6245(3) 0.73525(16) 0.66613(18) 0.0434(6) Uani 1 1 d . . .
C1 C 0.2486(4) 0.6096(2) 0.6058(2) 0.0438(7) Uani 1 1 d . . .
H1A H 0.162(3) 0.6256(18) 0.565(2) 0.042(8) Uiso 1 1 d . . .
H2B H 0.305(4) 0.571(2) 0.569(2) 0.051(10) Uiso 1 1 d . . .
C2 C 0.1985(3) 0.5686(2) 0.6947(2) 0.0406(7) Uani 1 1 d . . .
C3 C 0.0590(4) 0.5370(3) 0.7029(3) 0.0552(9) Uani 1 1 d . . .
H3 H -0.003(4) 0.542(2) 0.655(3) 0.062(11) Uiso 1 1 d . . .
C4 C 0.0221(4) 0.4969(3) 0.7840(3) 0.0616(10) Uani 1 1 d . . .
H4 H -0.075(5) 0.475(2) 0.792(3) 0.076(12) Uiso 1 1 d . . .
C5 C 0.1278(4) 0.4881(2) 0.8559(3) 0.0540(9) Uani 1 1 d . . .
H5 H 0.105(4) 0.461(2) 0.912(2) 0.049(9) Uiso 1 1 d . . .
C6 C 0.2652(4) 0.5210(2) 0.8432(2) 0.0427(7) Uani 1 1 d . . .
H6 H 0.349(4) 0.516(2) 0.894(3) 0.063(11) Uiso 1 1 d . . .
C7 C 0.2512(5) 0.7514(3) 0.6627(3) 0.0565(10) Uani 1 1 d . . .
H7A H 0.260(4) 0.799(2) 0.622(3) 0.075(12) Uiso 1 1 d . . .
H7B H 0.144(6) 0.740(3) 0.659(3) 0.109(17) Uiso 1 1 d . . .
C8 C 0.2793(3) 0.77931(18) 0.7632(2) 0.0397(7) Uani 1 1 d . . .
C9 C 0.1938(4) 0.8414(2) 0.7994(3) 0.0499(8) Uani 1 1 d . . .
H9 H 0.121(4) 0.864(2) 0.760(3) 0.059(10) Uiso 1 1 d . . .
C10 C 0.2213(4) 0.8698(2) 0.8892(3) 0.0577(10) Uani 1 1 d . . .
H10 H 0.165(4) 0.910(2) 0.911(2) 0.055(10) Uiso 1 1 d . . .
C11 C 0.3336(4) 0.8360(2) 0.9425(3) 0.0598(10) Uani 1 1 d . . .
H11 H 0.350(4) 0.852(2) 1.003(3) 0.060(11) Uiso 1 1 d . . .
C12 C 0.4130(4) 0.7734(2) 0.9040(3) 0.0532(9) Uani 1 1 d . . .
H12 H 0.488(4) 0.745(2) 0.936(3) 0.061(11) Uiso 1 1 d . . .
C13 C 0.4316(4) 0.7059(2) 0.5494(2) 0.0446(8) Uani 1 1 d . . .
H13A H 0.469(3) 0.6558(19) 0.520(2) 0.035(8) Uiso 1 1 d . . .
H13B H 0.373(3) 0.7344(19) 0.499(2) 0.048(9) Uiso 1 1 d . . .
C14 C 0.5601(3) 0.75784(18) 0.5829(2) 0.0412(7) Uani 1 1 d . . .
C15 C 0.6117(4) 0.8232(2) 0.5310(3) 0.0532(9) Uani 1 1 d . . .
H15 H 0.559(4) 0.836(2) 0.477(3) 0.062(11) Uiso 1 1 d . . .
C16 C 0.7309(5) 0.8664(2) 0.5650(3) 0.0633(10) Uani 1 1 d . . .
H16 H 0.764(5) 0.912(3) 0.530(3) 0.088(14) Uiso 1 1 d . . .
C17 C 0.7972(5) 0.8440(2) 0.6503(3) 0.0635(10) Uani 1 1 d . . .
H17 H 0.879(5) 0.872(3) 0.678(3) 0.080(13) Uiso 1 1 d . . .
C18 C 0.7411(4) 0.7787(2) 0.6987(3) 0.0558(9) Uani 1 1 d . . .
H18 H 0.783(4) 0.760(2) 0.756(2) 0.050(9) Uiso 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N4 Mn N2 146.47(9) . . ?
N4 Mn N3 84.06(10) . . ?
N2 Mn N3 86.53(9) . . ?
N4 Mn N1 73.15(9) . . ?
N2 Mn N1 73.32(9) . . ?
N3 Mn N1 74.56(9) . . ?
N4 Mn I1 107.02(7) . . ?
N2 Mn I1 105.57(6) . . ?
N3 Mn I1 93.06(6) . . ?
N1 Mn I1 167.59(6) . . ?
N4 Mn I2 91.80(7) . . ?
N2 Mn I2 92.33(7) . . ?
N3 Mn I2 170.53(6) . . ?
N1 Mn I2 96.10(6) . . ?
I1 Mn I2 96.297(18) . . ?
C13 N1 C1 111.5(2) . . ?
C13 N1 C7 111.9(3) . . ?
C1 N1 C7 111.2(3) . . ?
C13 N1 Mn 105.00(18) . . ?
C1 N1 Mn 104.99(17) . . ?
C7 N1 Mn 111.89(19) . . ?
C6 N2 C2 117.9(3) . . ?
C6 N2 Mn 125.3(2) . . ?
C2 N2 Mn 116.3(2) . . ?
C8 N3 C12 117.7(3) . . ?
C8 N3 Mn 117.1(2) . . ?
C12 N3 Mn 125.2(2) . . ?
C18 N4 C14 118.2(3) . . ?
C18 N4 Mn 124.9(2) . . ?
C14 N4 Mn 116.4(2) . . ?
N1 C1 C2 110.4(3) . . ?
N2 C2 C3 121.8(3) . . ?
N2 C2 C1 115.5(3) . . ?
C3 C2 C1 122.7(3) . . ?
C4 C3 C2 120.0(3) . . ?
C3 C4 C5 118.6(3) . . ?
C6 C5 C4 118.5(3) . . ?
N2 C6 C5 123.1(3) . . ?
N1 C7 C8 116.9(3) . . ?
N3 C8 C9 121.4(3) . . ?
N3 C8 C7 119.4(3) . . ?
C9 C8 C7 119.2(3) . . ?
C10 C9 C8 120.1(3) . . ?
C11 C10 C9 119.2(3) . . ?
C10 C11 C12 118.3(4) . . ?
N3 C12 C11 123.3(3) . . ?
N1 C13 C14 110.8(3) . . ?
N4 C14 C15 121.8(3) . . ?
N4 C14 C13 115.7(3) . . ?
C15 C14 C13 122.4(3) . . ?
C16 C15 C14 119.1(3) . . ?
C15 C16 C17 119.6(4) . . ?
C18 C17 C16 118.7(4) . . ?
N4 C18 C17 122.6(4) . . ?
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
Mn N4 2.263(3) . ?
Mn N2 2.267(2) . ?
Mn N3 2.318(3) . ?
Mn N1 2.363(2) . ?
Mn I1 2.8011(9) . ?
Mn I2 2.8773(7) . ?
N1 C13 1.474(4) . ?
N1 C1 1.476(4) . ?
N1 C7 1.479(4) . ?
N2 C6 1.339(4) . ?
N2 C2 1.346(4) . ?
N3 C8 1.334(4) . ?
N3 C12 1.354(4) . ?
N4 C18 1.343(4) . ?
N4 C14 1.348(4) . ?
C1 C2 1.505(4) . ?
C2 C3 1.379(4) . ?
C3 C4 1.369(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.377(5) . ?
C7 C8 1.506(5) . ?
C8 C9 1.382(4) . ?
C9 C10 1.367(5) . ?
C10 C11 1.366(5) . ?
C11 C12 1.370(5) . ?
C13 C14 1.506(4) . ?
C14 C15 1.381(4) . ?
C15 C16 1.366(5) . ?
C16 C17 1.380(6) . ?
C17 C18 1.369(5) . ?
