#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179118 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/80/4308036.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_4308036
loop_
_publ_author_name
'Sonia Nieto'
'Julio Pérez'
'Lucía Riera'
'Víctor Riera'
'Daniel Miguel'
'James A. Golen'
'Arnold L. Rheingold'
_publ_contact_author
;
     JULIO PEREZ
     Departamento de Quimica Organica e Inorganica 
     IUQOEM - Facultad de Quimica
     Universidad de Oviedo-CSIC
     C/ Julian Claveria s/n
     33006 Oviedo  (ASTURIAS)
     SPAIN
;
_publ_contact_author_email       japm@uniovi.es
_publ_contact_author_fax         +34-85-103446
_publ_contact_author_phone       +34-85-102985
_publ_section_title
;
Pyrazole Complexes as Anion Receptors: Effects of Changing the Metal, the
Pyrazole Substitution Pattern, and the Number of Pyrazole Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3407
_journal_page_last               3418
_journal_paper_doi               10.1021/ic0700046
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C18 H24 Mn N7 O6'
_chemical_formula_weight         489.38
_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                 110.941(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.865(3)
_cell_length_b                   14.837(4)
_cell_length_c                   14.004(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2302.4(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10229
_diffrn_reflns_theta_full        23.37
_diffrn_reflns_theta_max         23.37
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.698024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0405
_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)+(0.0652P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                2452
_reflns_number_total             3334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0700046si20070102_075057_04.cif
_cod_data_source_block           Compound_6_(sn309am)
_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        2302.6(11)
_cod_database_code               4308036
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.80881(4) 0.91716(3) 0.17252(3) 0.03727(19) Uani 1 1 d . . .
C1 C 0.9324(3) 0.9182(2) 0.2920(3) 0.0487(8) Uani 1 1 d . . .
O1 O 1.0094(3) 0.92360(19) 0.36996(19) 0.0770(8) Uani 1 1 d . . .
C2 C 0.7608(3) 1.0195(2) 0.2166(2) 0.0447(8) Uani 1 1 d . . .
O2 O 0.7396(2) 1.08485(17) 0.2505(2) 0.0700(8) Uani 1 1 d . . .
C3 C 0.8977(3) 0.9859(2) 0.1175(3) 0.0482(8) Uani 1 1 d . . .
O3 O 0.9570(3) 1.03118(19) 0.0899(2) 0.0786(8) Uani 1 1 d . . .
N1 N 0.8615(2) 0.79920(16) 0.12133(18) 0.0389(6) Uani 1 1 d . . .
N2 N 0.7799(3) 0.73282(17) 0.07727(18) 0.0409(6) Uani 1 1 d . . .
H2 H 0.693(3) 0.737(2) 0.067(2) 0.064(11) Uiso 1 1 d . . .
N3 N 0.7028(2) 0.84030(16) 0.23073(18) 0.0374(6) Uani 1 1 d . . .
N4 N 0.5878(2) 0.86865(19) 0.2146(2) 0.0370(6) Uani 1 1 d . . .
H4 H 0.560(3) 0.910(2) 0.175(2) 0.037(9) Uiso 1 1 d . . .
N5 N 0.6145(3) 0.96295(18) -0.0294(2) 0.0443(7) Uani 1 1 d . . .
O4 O 0.65759(18) 0.90479(13) 0.04208(14) 0.0387(5) Uani 1 1 d . . .
O5 O 0.5143(2) 0.94800(15) -0.09473(17) 0.0539(6) Uani 1 1 d . . .
O6 O 0.6685(3) 1.0319(2) -0.0301(2) 0.0922(11) Uani 1 1 d . . .
N7 N 0.5260(3) 0.70877(18) 0.0451(2) 0.0507(7) Uani 1 1 d . . .
N8 N 0.4321(3) 0.7637(2) -0.0074(2) 0.0471(7) Uani 1 1 d . . .
H8 H 0.449(3) 0.812(2) -0.033(2) 0.046(10) Uiso 1 1 d . . .
C11 C 0.9681(3) 0.7664(2) 0.1236(2) 0.0474(9) Uani 1 1 d . . .
C12 C 0.9527(3) 0.6802(2) 0.0828(3) 0.0560(9) Uani 1 1 d . . .
H12 H 1.0128 0.6430 0.0767 0.067 Uiso 1 1 calc R . .
C13 C 0.8332(3) 0.6605(2) 0.0536(2) 0.0496(9) Uani 1 1 d . . .
C14 C 1.0823(3) 0.8192(3) 0.1620(3) 0.0687(11) Uani 1 1 d . . .
H14A H 1.0785 0.8677 0.1155 0.103 Uiso 1 1 calc R . .
H14B H 1.1491 0.7806 0.1670 0.103 Uiso 1 1 calc R . .
H14C H 1.0928 0.8434 0.2282 0.103 Uiso 1 1 calc R . .
C15 C 0.7640(4) 0.5792(2) 0.0029(3) 0.0681(11) Uani 1 1 d . . .
H15A H 0.7762 0.5319 0.0524 0.102 Uiso 1 1 calc R . .
H15B H 0.7915 0.5595 -0.0503 0.102 Uiso 1 1 calc R . .
H15C H 0.6797 0.5937 -0.0259 0.102 Uiso 1 1 calc R . .
C21 C 0.7187(3) 0.7676(2) 0.2917(2) 0.0411(8) Uani 1 1 d . . .
C22 C 0.6131(3) 0.7516(2) 0.3116(2) 0.0458(8) Uani 1 1 d . . .
H22 H 0.6010 0.7056 0.3519 0.055 Uiso 1 1 calc R . .
C23 C 0.5314(3) 0.8155(2) 0.2613(2) 0.0402(8) Uani 1 1 d . . .
C24 C 0.8331(3) 0.7149(2) 0.3290(2) 0.0551(9) Uani 1 1 d . . .
H24A H 0.8383 0.6777 0.2747 0.083 Uiso 1 1 calc R . .
H24B H 0.8343 0.6777 0.3854 0.083 Uiso 1 1 calc R . .
H24C H 0.9005 0.7556 0.3509 0.083 Uiso 1 1 calc R . .
C25 C 0.4038(3) 0.8309(2) 0.2512(3) 0.0558(9) Uani 1 1 d . . .
H25A H 0.3607 0.7748 0.2365 0.084 Uiso 1 1 calc R . .
H25B H 0.3669 0.8727 0.1966 0.084 Uiso 1 1 calc R . .
H25C H 0.4014 0.8551 0.3140 0.084 Uiso 1 1 calc R . .
C31 C 0.4727(4) 0.6411(2) 0.0754(3) 0.0533(9) Uani 1 1 d . . .
C32 C 0.3496(4) 0.6534(2) 0.0418(3) 0.0573(10) Uani 1 1 d . . .
H32 H 0.2938 0.6152 0.0534 0.069 Uiso 1 1 calc R . .
C33 C 0.3250(3) 0.7325(2) -0.0120(3) 0.0484(9) Uani 1 1 d . . .
C34 C 0.5466(4) 0.5660(3) 0.1392(3) 0.0814(13) Uani 1 1 d . . .
H34A H 0.5359 0.5126 0.0983 0.122 Uiso 1 1 calc R . .
H34B H 0.5209 0.5546 0.1958 0.122 Uiso 1 1 calc R . .
H34C H 0.6302 0.5829 0.1645 0.122 Uiso 1 1 calc R . .
C35 C 0.2105(3) 0.7800(3) -0.0634(3) 0.0705(11) Uani 1 1 d . . .
H35A H 0.2138 0.8385 -0.0334 0.106 Uiso 1 1 calc R . .
H35B H 0.1454 0.7460 -0.0557 0.106 Uiso 1 1 calc R . .
H35C H 0.1976 0.7864 -0.1348 0.106 Uiso 1 1 calc R . .
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'
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
C1 Mn1 C2 85.75(15) . . ?
C1 Mn1 C3 89.17(15) . . ?
C2 Mn1 C3 88.56(14) . . ?
C1 Mn1 O4 173.43(12) . . ?
C2 Mn1 O4 95.57(12) . . ?
C3 Mn1 O4 97.30(12) . . ?
C1 Mn1 N3 92.71(12) . . ?
C2 Mn1 N3 91.03(12) . . ?
C3 Mn1 N3 178.05(13) . . ?
O4 Mn1 N3 80.84(9) . . ?
C1 Mn1 N1 94.79(13) . . ?
C2 Mn1 N1 179.23(12) . . ?
C3 Mn1 N1 92.01(12) . . ?
O4 Mn1 N1 83.84(9) . . ?
N3 Mn1 N1 88.39(10) . . ?
O1 C1 Mn1 176.1(3) . . ?
O2 C2 Mn1 174.4(3) . . ?
O3 C3 Mn1 175.2(3) . . ?
C11 N1 N2 105.0(3) . . ?
C11 N1 Mn1 134.0(2) . . ?
N2 N1 Mn1 120.9(2) . . ?
C13 N2 N1 111.5(3) . . ?
C21 N3 N4 104.9(2) . . ?
C21 N3 Mn1 136.4(2) . . ?
N4 N3 Mn1 118.48(18) . . ?
C23 N4 N3 112.3(3) . . ?
O6 N5 O5 121.2(3) . . ?
O6 N5 O4 120.8(3) . . ?
O5 N5 O4 117.9(3) . . ?
N5 O4 Mn1 127.62(19) . . ?
C31 N7 N8 103.5(3) . . ?
C33 N8 N7 113.5(3) . . ?
N1 C11 C12 109.9(3) . . ?
N1 C11 C14 123.0(3) . . ?
C12 C11 C14 127.1(3) . . ?
C13 C12 C11 107.0(3) . . ?
N2 C13 C12 106.6(3) . . ?
N2 C13 C15 122.4(3) . . ?
C12 C13 C15 131.0(3) . . ?
N3 C21 C22 109.3(3) . . ?
N3 C21 C24 123.1(3) . . ?
C22 C21 C24 127.7(3) . . ?
C23 C22 C21 107.6(3) . . ?
N4 C23 C22 105.9(3) . . ?
N4 C23 C25 122.0(3) . . ?
C22 C23 C25 132.0(3) . . ?
N7 C31 C32 110.9(3) . . ?
N7 C31 C34 120.4(4) . . ?
C32 C31 C34 128.7(3) . . ?
C33 C32 C31 107.1(3) . . ?
N8 C33 C32 105.0(3) . . ?
N8 C33 C35 123.8(3) . . ?
C32 C33 C35 131.2(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 C1 1.788(4) . ?
Mn1 C2 1.806(4) . ?
Mn1 C3 1.824(4) . ?
Mn1 O4 2.061(2) . ?
Mn1 N3 2.069(2) . ?
Mn1 N1 2.071(3) . ?
C1 O1 1.149(4) . ?
C2 O2 1.146(4) . ?
C3 O3 1.136(4) . ?
N1 C11 1.345(4) . ?
N1 N2 1.364(3) . ?
N2 C13 1.346(4) . ?
N3 C21 1.346(4) . ?
N3 N4 1.367(3) . ?
N4 C23 1.345(4) . ?
N5 O6 1.209(3) . ?
N5 O5 1.234(3) . ?
N5 O4 1.281(3) . ?
N7 C31 1.334(4) . ?
N7 N8 1.364(4) . ?
N8 C33 1.332(4) . ?
C11 C12 1.386(5) . ?
C11 C14 1.489(5) . ?
C12 C13 1.360(5) . ?
C13 C15 1.489(5) . ?
C21 C22 1.397(4) . ?
C21 C24 1.490(4) . ?
C22 C23 1.358(4) . ?
C23 C25 1.488(4) . ?
C31 C32 1.377(5) . ?
C31 C34 1.499(5) . ?
C32 C33 1.369(5) . ?
C33 C35 1.470(5) . ?
