#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307873.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_4307873
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 Br2 Mn N4'
_chemical_formula_weight         505.12
_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                 96.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0109(18)
_cell_length_b                   15.951(3)
_cell_length_c                   13.459(3)
_cell_measurement_temperature    193(2)
_cell_volume                     1922.7(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      193(2)
_diffrn_measured_fraction_theta_full 0.803
_diffrn_measured_fraction_theta_max 0.803
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7395
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.851
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.630
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0352
_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)+(0.0607P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                3295
_reflns_number_total             4003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062384l-file003.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        1922.8(7)
_cod_database_code               4307873
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
Mn1 Mn 1.01230(5) 0.12805(3) 0.24518(3) 0.01984(12) Uani 1 1 d . . .
N1 N 0.8323(3) 0.17735(15) 0.11655(17) 0.0209(5) Uani 1 1 d . . .
N2 N 0.7988(3) 0.05452(15) 0.25759(17) 0.0223(5) Uani 1 1 d . . .
N3 N 0.8840(3) 0.23531(15) 0.31598(18) 0.0234(6) Uani 1 1 d . . .
N4 N 1.1183(3) 0.23462(15) 0.16684(19) 0.0250(6) Uani 1 1 d . . .
C1 C 0.7385(4) 0.1028(2) 0.0880(2) 0.0256(7) Uani 1 1 d . . .
H1A H 0.795(4) 0.0662(19) 0.054(2) 0.019(8) Uiso 1 1 d . . .
H1B H 0.646(4) 0.1185(18) 0.041(2) 0.015(7) Uiso 1 1 d . . .
C2 C 0.6905(4) 0.06245(19) 0.1807(2) 0.0243(7) Uani 1 1 d . . .
C3 C 0.5470(4) 0.0341(2) 0.1868(3) 0.0326(8) Uani 1 1 d . . .
H3 H 0.476(4) 0.042(2) 0.136(2) 0.020(8) Uiso 1 1 d . . .
C4 C 0.5120(5) -0.0033(2) 0.2732(3) 0.0378(9) Uani 1 1 d . . .
H4 H 0.420(5) -0.023(3) 0.277(4) 0.061(14) Uiso 1 1 d . . .
C5 C 0.6226(4) -0.0137(2) 0.3516(2) 0.0307(8) Uani 1 1 d . . .
H5 H 0.598(5) -0.040(3) 0.414(4) 0.063(13) Uiso 1 1 d . . .
C6 C 0.7656(4) 0.01553(19) 0.3413(2) 0.0256(7) Uani 1 1 d . . .
H6 H 0.851(4) 0.013(2) 0.399(3) 0.032(9) Uiso 1 1 d . . .
C11 C 0.7418(4) 0.2475(2) 0.1492(2) 0.0286(7) Uani 1 1 d . . .
H11A H 0.642(4) 0.229(2) 0.134(3) 0.041(11) Uiso 1 1 d . . .
H11B H 0.758(4) 0.295(2) 0.113(3) 0.042(11) Uiso 1 1 d . . .
C12 C 0.7746(3) 0.27330(18) 0.2572(2) 0.0220(6) Uani 1 1 d . . .
C13 C 0.6896(4) 0.3375(2) 0.2936(3) 0.0305(7) Uani 1 1 d . . .
H13 H 0.608(5) 0.361(2) 0.251(3) 0.040(11) Uiso 1 1 d . . .
C14 C 0.7189(4) 0.3628(2) 0.3922(3) 0.0334(8) Uani 1 1 d . . .
H14 H 0.657(4) 0.407(3) 0.413(3) 0.047(12) Uiso 1 1 d . . .
C15 C 0.8313(4) 0.3236(2) 0.4524(3) 0.0319(8) Uani 1 1 d . . .
H15 H 0.855(4) 0.334(2) 0.518(3) 0.040(11) Uiso 1 1 d . . .
C16 C 0.9106(4) 0.2608(2) 0.4123(2) 0.0279(7) Uani 1 1 d . . .
H16 H 0.977(4) 0.234(2) 0.447(3) 0.025(9) Uiso 1 1 d . . .
C21 C 0.9205(4) 0.20345(19) 0.0354(2) 0.0252(7) Uani 1 1 d . . .
H21A H 0.857(4) 0.232(2) -0.024(3) 0.031(9) Uiso 1 1 d . . .
H21B H 0.965(3) 0.1508(19) 0.012(2) 0.017(8) Uiso 1 1 d . . .
C22 C 1.0487(3) 0.25803(18) 0.0775(2) 0.0226(6) Uani 1 1 d . . .
C23 C 1.0942(4) 0.32764(19) 0.0267(2) 0.0275(7) Uani 1 1 d . . .
H23 H 1.031(4) 0.347(2) -0.029(2) 0.020(8) Uiso 1 1 d . . .
C24 C 1.2130(4) 0.3750(2) 0.0696(3) 0.0328(8) Uani 1 1 d . . .
H24 H 1.251(4) 0.420(2) 0.035(3) 0.040(10) Uiso 1 1 d . . .
C25 C 1.2842(4) 0.3513(2) 0.1618(3) 0.0336(8) Uani 1 1 d . . .
H25 H 1.351(5) 0.383(2) 0.194(3) 0.046(12) Uiso 1 1 d . . .
C26 C 1.2341(4) 0.2808(2) 0.2070(3) 0.0303(7) Uani 1 1 d . . .
H26 H 1.276(4) 0.262(2) 0.264(3) 0.034(10) Uiso 1 1 d . . .
Br2 Br 1.12336(4) 0.01422(2) 0.13423(2) 0.02701(11) Uani 1 1 d . . .
Br1 Br 1.18285(4) 0.10301(2) 0.40910(2) 0.03241(11) 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'
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
N4 Mn1 N2 145.49(10) . . ?
N4 Mn1 N3 83.84(9) . . ?
N2 Mn1 N3 83.50(9) . . ?
N4 Mn1 N1 72.61(9) . . ?
N2 Mn1 N1 73.07(9) . . ?
N3 Mn1 N1 74.01(9) . . ?
N4 Mn1 Br1 105.81(7) . . ?
N2 Mn1 Br1 106.65(7) . . ?
N3 Mn1 Br1 92.27(7) . . ?
N1 Mn1 Br1 166.26(6) . . ?
N4 Mn1 Br2 92.74(7) . . ?
N2 Mn1 Br2 93.66(6) . . ?
N3 Mn1 Br2 169.02(7) . . ?
N1 Mn1 Br2 95.01(6) . . ?
Br1 Mn1 Br2 98.71(2) . . ?
C21 N1 C11 111.4(2) . . ?
C21 N1 C1 111.8(2) . . ?
C11 N1 C1 111.5(3) . . ?
C21 N1 Mn1 104.59(19) . . ?
C11 N1 Mn1 112.87(18) . . ?
C1 N1 Mn1 104.33(18) . . ?
C2 N2 C6 118.4(3) . . ?
C2 N2 Mn1 116.21(19) . . ?
C6 N2 Mn1 124.5(2) . . ?
C12 N3 C16 118.1(3) . . ?
C12 N3 Mn1 117.23(19) . . ?
C16 N3 Mn1 124.7(2) . . ?
C26 N4 C22 118.2(3) . . ?
C26 N4 Mn1 125.0(2) . . ?
C22 N4 Mn1 116.4(2) . . ?
N1 C1 C2 109.5(2) . . ?
N2 C2 C3 121.8(3) . . ?
N2 C2 C1 115.2(3) . . ?
C3 C2 C1 123.0(3) . . ?
C4 C3 C2 119.7(3) . . ?
C3 C4 C5 119.1(3) . . ?
C4 C5 C6 118.8(3) . . ?
N2 C6 C5 122.1(3) . . ?
N1 C11 C12 115.9(3) . . ?
N3 C12 C13 121.4(3) . . ?
N3 C12 C11 120.0(3) . . ?
C13 C12 C11 118.7(3) . . ?
C14 C13 C12 119.7(3) . . ?
C15 C14 C13 118.8(3) . . ?
C14 C15 C16 118.8(3) . . ?
N3 C16 C15 123.3(3) . . ?
N1 C21 C22 109.8(2) . . ?
N4 C22 C23 121.8(3) . . ?
N4 C22 C21 115.9(3) . . ?
C23 C22 C21 122.2(3) . . ?
C24 C23 C22 119.2(3) . . ?
C23 C24 C25 119.0(3) . . ?
C26 C25 C24 118.4(3) . . ?
N4 C26 C25 123.3(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 N4 2.266(3) . ?
Mn1 N2 2.275(3) . ?
Mn1 N3 2.327(2) . ?
Mn1 N1 2.372(3) . ?
Mn1 Br1 2.5771(10) . ?
Mn1 Br2 2.6187(7) . ?
N1 C21 1.479(4) . ?
N1 C11 1.480(4) . ?
N1 C1 1.484(4) . ?
N2 C2 1.348(4) . ?
N2 C6 1.350(4) . ?
N3 C12 1.339(4) . ?
N3 C16 1.355(4) . ?
N4 C26 1.341(4) . ?
N4 C22 1.347(4) . ?
C1 C2 1.509(4) . ?
C2 C3 1.381(5) . ?
C3 C4 1.375(5) . ?
C4 C5 1.379(5) . ?
C5 C6 1.391(5) . ?
C11 C12 1.508(4) . ?
C12 C13 1.400(4) . ?
C13 C14 1.385(5) . ?
C14 C15 1.375(5) . ?
C15 C16 1.375(5) . ?
C21 C22 1.506(4) . ?
C22 C23 1.389(4) . ?
C23 C24 1.384(5) . ?
C24 C25 1.386(5) . ?
C25 C26 1.379(5) . ?
