#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332476.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332476
loop_
_publ_author_name
'Choi, Da Hye'
'Yoon, Jung Hee'
'Lim, Jeong Hak'
'Kim, Hyoung Chan'
'Hong, Chang Seop'
_publ_section_title
;
 Methylpyrazole-Capped Two-Dimensional Supramolecular M(II) (M = Mn, Ni,
 Co) Assemblies Constructed by Covalent and Noncovalent
 Interactions:  Uncommon Coordination Modes of Methylpyrazoles and
 Magnetic Properties
;
_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5947
_journal_page_last               5952
_journal_paper_doi               10.1021/ic060429c
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C8 H12 Mn0.5 N7'
_chemical_formula_weight         233.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8530(10)
_cell_length_b                   9.0560(10)
_cell_length_c                   14.884(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1154.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.854
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1730
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.605
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             486
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0369
_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)+(0.0479P)²+0.3968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                1376
_reflns_number_total             1730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060429csup1.cif
_cod_data_source_block           mn
_cod_original_cell_volume        1154.4(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C8 H12 Mn0.50 N7'
_cod_database_code               4332476
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mn1 Mn 1.0000 0.5000 0.5000 0.0440(2) Uani 1 2 d S
N5 N 0.9325(4) 0.5040(3) 0.63310(18) 0.0688(8) Uani 1 1 d .
N6 N 0.9392(3) 0.4171(3) 0.69107(18) 0.0591(7) Uani 1 1 d .
N7 N 0.9475(5) 0.3308(4) 0.7497(2) 0.1029(13) Uani 1 1 d .
N1 N 0.7670(3) 0.4029(3) 0.42401(18) 0.0564(7) Uani 1 1 d .
N2 N 0.7350(3) 0.3301(3) 0.34246(18) 0.0584(7) Uani 1 1 d .
H2 H 0.8027 0.3154 0.3110 0.070 Uiso 1 1 calc .
C1 C 0.6339(4) 0.4009(4) 0.4482(3) 0.0786(11) Uani 1 1 d .
H1 H 0.6188 0.4426 0.5023 0.094 Uiso 1 1 calc .
C2 C 0.5187(4) 0.3281(5) 0.3820(4) 0.0937(13) Uani 1 1 d .
H2C H 0.4154 0.3135 0.3834 0.112 Uiso 1 1 calc .
C3 C 0.5870(4) 0.2829(4) 0.3154(3) 0.0713(10) Uani 1 1 d .
C4 C 0.5287(6) 0.1970(5) 0.2268(3) 0.1122(17) Uani 1 1 d .
H4A H 0.6117 0.1854 0.1966 0.168 Uiso 1 1 calc .
H4B H 0.4436 0.2492 0.1865 0.168 Uiso 1 1 calc .
H4C H 0.4935 0.1015 0.2408 0.168 Uiso 1 1 calc .
N3 N 1.1024 0.2696 0.5204 0.052 Uani 1 1 d .
N4 N 1.1422 0.1976 0.4502 0.059 Uani 1 1 d .
H4 H 1.1282 0.2327 0.3951 0.071 Uiso 1 1 calc .
C5 C 1.1426(4) 0.1775(4) 0.5906(2) 0.0702(10) Uani 1 1 d .
H5 H 1.1285 0.1959 0.6494 0.084 Uiso 1 1 calc .
C6 C 1.2084(5) 0.0499(4) 0.5665(3) 0.0833(12) Uani 1 1 d .
H6 H 1.2466 -0.0299 0.6048 0.100 Uiso 1 1 calc .
C7 C 1.2060(4) 0.0649(4) 0.4765(3) 0.0675(9) Uani 1 1 d .
C8 C 1.2581(6) -0.0340(4) 0.4091(4) 0.1039(15) Uani 1 1 d .
H8A H 1.2381 0.0134 0.3495 0.156 Uiso 1 1 calc .
H8B H 1.2017 -0.1255 0.4033 0.156 Uiso 1 1 calc .
H8C H 1.3679 -0.0532 0.4313 0.156 Uiso 1 1 calc .
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'
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
N5 Mn1 N5 180.0 . 3_766
N5 Mn1 N1 87.99(11) . 3_766
N5 Mn1 N1 92.01(11) 3_766 3_766
N5 Mn1 N1 92.01(11) . .
N5 Mn1 N1 87.99(11) 3_766 .
N1 Mn1 N1 180.0 3_766 .
N5 Mn1 N3 85.15(7) . 3_766
N5 Mn1 N3 94.85(7) 3_766 3_766
N1 Mn1 N3 89.56(6) 3_766 3_766
N1 Mn1 N3 90.44(6) . 3_766
N5 Mn1 N3 94.85(7) . .
N5 Mn1 N3 85.15(7) 3_766 .
N1 Mn1 N3 90.44(6) 3_766 .
N1 Mn1 N3 89.56(6) . .
N3 Mn1 N3 180.0 3_766 .
N6 N5 Mn1 133.0(2) . .
N5 N6 N7 179.2(4) . .
C1 N1 N2 104.0(3) . .
C1 N1 Mn1 129.4(2) . .
N2 N1 Mn1 126.67(19) . .
C3 N2 N1 113.2(3) . .
N1 C1 C2 111.0(4) . .
C3 C2 C1 106.3(3) . .
N2 C3 C2 105.5(3) . .
N2 C3 C4 121.4(4) . .
C2 C3 C4 133.0(4) . .
C5 N3 N4 103.71(16) . .
C5 N3 Mn1 135.28(16) . .
N4 N3 Mn1 121.0 . .
C7 N4 N3 112.31(18) . .
N3 C5 C6 111.8(3) . .
C7 C6 C5 105.9(3) . .
C6 C7 N4 106.3(3) . .
C6 C7 C8 132.6(4) . .
N4 C7 C8 121.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N5 2.210(2) .
Mn1 N5 2.210(2) 3_766
Mn1 N1 2.264(3) 3_766
Mn1 N1 2.264(3) .
Mn1 N3 2.2644 3_766
Mn1 N3 2.2644 .
N5 N6 1.158(3) .
N6 N7 1.160(4) .
N1 C1 1.316(4) .
N1 N2 1.347(3) .
N2 C3 1.339(4) .
C1 C2 1.392(5) .
C2 C3 1.349(6) .
C3 C4 1.505(6) .
N3 C5 1.314(3) .
N3 N4 1.3521 .
N4 C7 1.343(3) .
C5 C6 1.382(5) .
C6 C7 1.340(5) .
C7 C8 1.502(6) .
