#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:40:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179388 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/85/4328512.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_4328512
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_formula_sum            'C17 H19 Cl Mn N3 O7'
_chemical_formula_weight         467.74
_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                 94.857(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.097(5)
_cell_length_b                   9.335(2)
_cell_length_c                   9.501(2)
_cell_measurement_reflns_used    895
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.614
_cell_measurement_theta_min      2.850
_cell_volume                     2129.5(8)
_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      298(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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16684
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.748043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0415
_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)+(0.0739P)²+0.3341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                2900
_reflns_number_total             3921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022984_si_002_04.cif
_cod_data_source_block           Compound_3b_rg695c
_cod_database_code               4328512
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 0.674343(18) 0.54685(4) 0.70841(5) 0.03820(17) Uani 1 1 d .
Cl1 Cl 0.60223(3) 0.53045(7) 0.86647(8) 0.0455(2) Uani 1 1 d .
N1 N 0.61355(10) 0.5139(2) 0.5475(2) 0.0383(5) Uani 1 1 d .
N2 N 0.67079(9) 0.3293(2) 0.7000(2) 0.0328(5) Uani 1 1 d .
N5 N 0.80610(11) 0.2219(3) 0.8329(3) 0.0538(7) Uani 1 1 d .
H5 H 0.8001 0.2286 0.9206 0.065 Uiso 1 1 calc R
C1 C 0.72739(14) 0.5579(3) 0.5864(4) 0.0501(8) Uani 1 1 d .
O1 O 0.76034(13) 0.5690(3) 0.5079(3) 0.0782(8) Uani 1 1 d .
C2 C 0.72637(15) 0.5602(3) 0.8583(4) 0.0545(8) Uani 1 1 d .
O2 O 0.75866(12) 0.5748(3) 0.9522(3) 0.0845(9) Uani 1 1 d .
C3 C 0.67030(13) 0.7403(4) 0.7104(3) 0.0508(8) Uani 1 1 d .
O3 O 0.66967(11) 0.8622(3) 0.7143(3) 0.0747(8) Uani 1 1 d .
C11 C 0.58565(13) 0.6127(3) 0.4678(3) 0.0497(8) Uani 1 1 d .
H11 H 0.5936 0.7090 0.4850 0.060 Uiso 1 1 calc R
C12 C 0.54575(15) 0.5775(4) 0.3615(4) 0.0608(9) Uani 1 1 d .
H12 H 0.5273 0.6493 0.3083 0.073 Uiso 1 1 calc R
C13 C 0.53323(15) 0.4371(4) 0.3340(4) 0.0602(9) Uani 1 1 d .
H13 H 0.5063 0.4119 0.2624 0.072 Uiso 1 1 calc R
C14 C 0.56151(13) 0.3334(3) 0.4151(3) 0.0515(8) Uani 1 1 d .
H14 H 0.5539 0.2368 0.3993 0.062 Uiso 1 1 calc R
C15 C 0.60129(11) 0.3752(3) 0.5201(3) 0.0376(6) Uani 1 1 d .
C16 C 0.63447(11) 0.2754(3) 0.6095(3) 0.0368(6) Uani 1 1 d .
H16 H 0.6295 0.1768 0.6011 0.044 Uiso 1 1 calc R
C4 C 0.70635(12) 0.2317(3) 0.7876(3) 0.0389(6) Uani 1 1 d .
H4A H 0.6903 0.1363 0.7835 0.047 Uiso 1 1 calc R
H4B H 0.7088 0.2636 0.8851 0.047 Uiso 1 1 calc R
C5 C 0.76396(12) 0.2278(3) 0.7353(3) 0.0391(7) Uani 1 1 d .
O5 O 0.76964(9) 0.2240(3) 0.6091(2) 0.0569(6) Uani 1 1 d .
C6 C 0.86220(15) 0.2043(5) 0.7939(4) 0.0734(12) Uani 1 1 d .
H6A H 0.8635 0.1180 0.7375 0.088 Uiso 1 1 calc R
H6B H 0.8864 0.1893 0.8795 0.088 Uiso 1 1 calc R
C7 C 0.88497(18) 0.3223(6) 0.7153(5) 0.0806(13) Uani 1 1 d .
O6 O 0.92009(14) 0.3084(5) 0.6345(4) 0.1290(15) Uani 1 1 d .
O7 O 0.86374(16) 0.4460(4) 0.7417(4) 0.1138(12) Uani 1 1 d .
H7 H 0.8780 0.5079 0.6952 0.171 Uiso 1 1 calc R
O90 O 0.9094(2) 0.6554(6) 0.6032(10) 0.241(4) Uani 1 1 d .
C91 C 0.9634(3) 0.6678(9) 0.5826(10) 0.170(4) Uani 1 1 d .
H91A H 0.9721 0.6145 0.4996 0.204 Uiso 1 1 calc R
H91B H 0.9865 0.6326 0.6638 0.204 Uiso 1 1 calc R
C92 C 0.9719(4) 0.8174(11) 0.5633(13) 0.193(4) Uani 1 1 d .
H92A H 0.9993 0.8531 0.6357 0.232 Uiso 1 1 calc R
H92B H 0.9856 0.8347 0.4718 0.232 Uiso 1 1 calc R
C93 C 0.9235(5) 0.8846(9) 0.5717(13) 0.215(5) Uani 1 1 d .
H93A H 0.9149 0.9428 0.4881 0.259 Uiso 1 1 calc R
H93B H 0.9257 0.9469 0.6537 0.259 Uiso 1 1 calc R
C94 C 0.8826(3) 0.7834(11) 0.5826(14) 0.235(6) Uani 1 1 d .
H94A H 0.8610 0.8051 0.6615 0.282 Uiso 1 1 calc R
H94B H 0.8578 0.7808 0.4969 0.282 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'
Cl Cl 0.1484 0.1585 '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
C1 Mn1 C3 89.51(14)
C1 Mn1 C2 91.18(16)
C3 Mn1 C2 87.58(14)
C1 Mn1 N2 93.53(12)
C3 Mn1 N2 174.39(12)
C2 Mn1 N2 97.06(12)
C1 Mn1 N1 91.71(13)
C3 Mn1 N1 96.99(12)
C2 Mn1 N1 174.61(12)
N2 Mn1 N1 78.22(9)
C1 Mn1 Cl1 178.68(11)
C3 Mn1 Cl1 90.85(11)
C2 Mn1 Cl1 90.10(12)
N2 Mn1 Cl1 86.01(6)
N1 Mn1 Cl1 86.98(7)
C11 N1 C15 117.5(3)
C11 N1 Mn1 127.7(2)
C15 N1 Mn1 114.79(19)
C16 N2 C4 118.2(2)
C16 N2 Mn1 116.37(18)
C4 N2 Mn1 125.40(17)
C5 N5 C6 120.5(3)
O1 C1 Mn1 177.8(3)
O2 C2 Mn1 177.1(3)
O3 C3 Mn1 177.4(3)
N1 C11 C12 122.5(3)
C13 C12 C11 120.0(3)
C12 C13 C14 118.4(3)
C15 C14 C13 119.0(3)
N1 C15 C14 122.6(3)
N1 C15 C16 113.7(2)
C14 C15 C16 123.7(3)
N2 C16 C15 116.9(2)
N2 C4 C5 109.7(2)
O5 C5 N5 123.2(3)
O5 C5 C4 120.4(3)
N5 C5 C4 116.3(2)
N5 C6 C7 116.5(3)
O6 C7 O7 122.3(5)
O6 C7 C6 124.1(5)
O7 C7 C6 113.6(4)
C91 O90 C94 110.9(6)
O90 C91 C92 104.9(6)
C93 C92 C91 108.5(7)
C92 C93 C94 108.5(8)
O90 C94 C93 106.3(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 C1 1.800(4)
Mn1 C3 1.809(3)
Mn1 C2 1.820(4)
Mn1 N2 2.034(2)
Mn1 N1 2.049(2)
Mn1 Cl1 2.3958(9)
N1 C11 1.338(4)
N1 C15 1.349(4)
N2 C16 1.277(3)
N2 C4 1.462(3)
N5 C5 1.317(4)
N5 C6 1.441(4)
C1 O1 1.139(4)
C2 O2 1.141(4)
C3 O3 1.139(4)
C11 C12 1.374(5)
C12 C13 1.365(5)
C13 C14 1.381(5)
C14 C15 1.380(4)
C15 C16 1.454(4)
C4 C5 1.514(4)
C5 O5 1.220(3)
C6 C7 1.463(6)
C7 O6 1.197(5)
C7 O7 1.295(6)
O90 C91 1.337(7)
O90 C94 1.364(9)
C91 C92 1.426(9)
C92 C93 1.332(10)
C93 C94 1.375(11)
