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#$Date: 2016-03-23 16:40:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179388 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/85/4328509.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_4328509
loop_
_publ_author_name
'Celedonio M. Álvarez'
'Raúl García-Rodríguez'
'Daniel Miguel'
_publ_contact_author
;
     DANIEL MIGUEL
     IU CINQUIMA/Quimica Inorganica
     Facultad de Ciencias
     Universidad de Valladolid
     C/ Prado de la Magdalena s/n
     47005 Valladolid
     SPAIN
;
_publ_contact_author_email       dmsj@qi.uva.es
_publ_contact_author_fax         +34-983-423013
_publ_contact_author_phone       +34-983-184096
_publ_section_title
;
 Iminopyridine Complexes of Manganese, Rhenium, and Molybdenum Derived
 from Amino Ester Methylserine and Peptides Gly-Gly, Gly-Val, and
 Gly-Gly-Gly: Self-Assembly of the Peptide Chains
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2984
_journal_page_last               2996
_journal_paper_doi               10.1021/ic2022984
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C13 H12 Br0.41 Cl0.59 Mn N2 O6'
_chemical_formula_weight         400.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 98.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.772(18)
_cell_length_b                   6.835(6)
_cell_length_c                   11.481(10)
_cell_measurement_reflns_used    647
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.102
_cell_measurement_theta_min      2.546
_cell_volume                     1536(2)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5006
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.048
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.621069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             804.8
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0914P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                1599
_reflns_number_total             2201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022984_si_002_01.cif
_cod_data_source_block           Compound_2a_rg70a
_cod_database_code               4328509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-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
Br1 Br 0.59181(8) 0.52403(13) 0.44265(11) 0.0486(6) Uani 0.406(8) 1 d PG
Mn1 Mn 0.58535(8) 0.6597(3) 0.23863(10) 0.0504(6) Uani 1 1 d G
Cl1 Cl 0.59427(8) 0.5288(4) 0.43261(13) 0.0486(6) Uani 0.594(8) 1 d PG
N1 N 0.5014(4) 0.7972(14) 0.2749(6) 0.051(2) Uani 1 1 d .
N2 N 0.6255(4) 0.9110(12) 0.3120(6) 0.044(2) Uani 1 1 d .
C1 C 0.5784(6) 0.754(2) 0.1003(11) 0.066(3) Uani 1 1 d .
O1 O 0.5758(5) 0.8028(19) 0.0063(8) 0.115(4) Uani 1 1 d .
C2 C 0.5417(6) 0.448(2) 0.1802(10) 0.066(3) Uani 1 1 d .
O2 O 0.5141(5) 0.3171(16) 0.1389(8) 0.108(4) Uani 1 1 d .
C3 C 0.6611(6) 0.5489(19) 0.2170(9) 0.060(3) Uani 1 1 d .
O3 O 0.7107(5) 0.4742(13) 0.1974(9) 0.091(3) Uani 1 1 d .
C4 C 0.6967(5) 0.9653(14) 0.3338(9) 0.046(3) Uani 1 1 d .
H4 H 0.6991 1.0969 0.3679 0.055 Uiso 1 1 calc R
C5 C 0.7266(7) 0.9763(17) 0.2213(11) 0.065(3) Uani 1 1 d .
O5 O 0.7819(5) 0.9302(17) 0.2105(9) 0.106(4) Uani 1 1 d .
C6 C 0.7018(11) 1.098(3) 0.0249(12) 0.158(9) Uani 1 1 d .
H6A H 0.7125 1.2343 0.0197 0.238 Uiso 1 1 calc R
H6B H 0.6643 1.0656 -0.0347 0.238 Uiso 1 1 calc R
H6C H 0.7409 1.0211 0.0137 0.238 Uiso 1 1 calc R
O6 O 0.6829(5) 1.0567(13) 0.1402(7) 0.077(2) Uani 1 1 d .
O7 O 0.7122(4) 0.8299(11) 0.5253(6) 0.066(2) Uani 1 1 d .
H7 H 0.6847 0.7514 0.5156 0.099 Uiso 1 1 d R
C7 C 0.7375(5) 0.8350(17) 0.4194(8) 0.053(3) Uani 1 1 d .
H7A H 0.7373 0.7038 0.3872 0.064 Uiso 1 1 calc R
H7B H 0.7844 0.8805 0.4326 0.064 Uiso 1 1 calc R
C11 C 0.4373(6) 0.741(2) 0.2583(9) 0.071(4) Uani 1 1 d .
H11 H 0.4270 0.6159 0.2287 0.085 Uiso 1 1 calc R
C12 C 0.3856(6) 0.857(3) 0.2829(12) 0.083(4) Uani 1 1 d .
H12 H 0.3408 0.8133 0.2658 0.100 Uiso 1 1 calc R
C13 C 0.3969(7) 1.024(3) 0.3284(14) 0.093(4) Uani 1 1 d .
H13 H 0.3606 1.1006 0.3449 0.112 Uiso 1 1 calc R
C14 C 0.4625(7) 1.093(2) 0.3537(10) 0.077(4) Uani 1 1 d .
H14 H 0.4723 1.2144 0.3884 0.093 Uiso 1 1 calc R
C15 C 0.5137(5) 0.9693(18) 0.3243(10) 0.057(3) Uani 1 1 d .
C16 C 0.5834(5) 1.0245(17) 0.3471(8) 0.052(2) Uani 1 1 d .
H16 H 0.5971 1.1400 0.3863 0.062 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'
Br Br -0.2901 2.4595 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Mn1 C3 89.3(6)
C1 Mn1 C2 89.2(5)
C3 Mn1 C2 88.5(5)
C1 Mn1 N1 93.3(5)
C3 Mn1 N1 175.6(4)
C2 Mn1 N1 95.1(5)
C1 Mn1 N2 92.4(5)
C3 Mn1 N2 97.7(4)
C2 Mn1 N2 173.6(4)
N1 Mn1 N2 78.6(3)
C1 Mn1 Cl1 179.6(5)
C3 Mn1 Cl1 91.1(4)
C2 Mn1 Cl1 90.9(4)
N1 Mn1 Cl1 86.3(2)
N2 Mn1 Cl1 87.5(2)
C1 Mn1 Br1 178.2(4)
C3 Mn1 Br1 92.4(4)
C2 Mn1 Br1 90.5(4)
N1 Mn1 Br1 85.0(2)
N2 Mn1 Br1 87.7(2)
Cl1 Mn1 Br1 1.4
C11 N1 C15 116.2(10)
C11 N1 Mn1 130.0(9)
C15 N1 Mn1 113.7(7)
C16 N2 C4 117.7(9)
C16 N2 Mn1 114.9(7)
C4 N2 Mn1 127.3(6)
O1 C1 Mn1 174.5(14)
O2 C2 Mn1 177.3(11)
O3 C3 Mn1 177.0(10)
N2 C4 C7 112.8(8)
N2 C4 C5 111.0(9)
C7 C4 C5 111.0(9)
O5 C5 O6 125.4(13)
O5 C5 C4 124.9(13)
O6 C5 C4 109.6(11)
C5 O6 C6 120.2(13)
O7 C7 C4 111.6(8)
N1 C11 C12 122.5(13)
C13 C12 C11 121.5(13)
C12 C13 C14 120.3(13)
C13 C14 C15 115.9(13)
N1 C15 C14 123.4(11)
N1 C15 C16 115.7(9)
C14 C15 C16 120.9(12)
N2 C16 C15 116.9(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br1 Mn1 2.5055
Mn1 C1 1.702(13)
Mn1 C3 1.728(13)
Mn1 C2 1.765(13)
Mn1 N1 2.002(9)
Mn1 N2 2.026(8)
Mn1 Cl1 2.3830
N1 C11 1.312(13)
N1 C15 1.313(13)
N2 C16 1.246(11)
N2 C4 1.442(12)
C1 O1 1.123(13)
C2 O2 1.120(13)
C3 O3 1.156(13)
C4 C7 1.479(13)
C4 C5 1.497(15)
C5 O5 1.162(13)
C5 O6 1.299(13)
C6 O6 1.453(13)
O7 C7 1.379(11)
C11 C12 1.359(18)
C12 C13 1.26(2)
C13 C14 1.373(19)
C14 C15 1.395(15)
C15 C16 1.418(14)
