#------------------------------------------------------------------------------
#$Date: 2018-09-03 19:38:49 +0300 (Mon, 03 Sep 2018) $
#$Revision: 210357 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/98/7029870.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_7029870
loop_
_publ_author_name
'Chaignon, Jérémy'
'Stiriba, Salah-Eddine'
'Lloret, Francisco'
'Yuste, Consuelo'
'Pilet, Guillaume'
'Bonneviot, Laurent'
'Albela, Belén'
'Castro, Isabel'
_publ_section_title
;
 Bioinspired manganese(ii) complexes with a clickable ligand for
 immobilisation on a solid support.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9704
_journal_page_last               9713
_journal_paper_doi               10.1039/c3dt53636j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H32 MN2 N20'
_chemical_formula_sum            'C28 H32 Mn2 N22'
_chemical_formula_weight         758.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 95.592(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.2568(3)
_cell_length_b                   18.4512(6)
_cell_length_c                   18.6889(6)
_cell_measurement_reflns_used    11318
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     3520.05(19)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23027
_diffrn_reflns_theta_full        25.132
_diffrn_reflns_theta_max         29.223
_diffrn_reflns_theta_min         3.024
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat lozenge'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.569
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3425
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0008774
_refine_ls_shift/su_mean         0.0000290
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.27 1.41 3.41 0.823 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0447
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0353
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                3649
_reflns_number_total             4407
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0312
_oxford_refine_ls_scale          1.2562(18)
_oxford_reflns_number_all        4398
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3dt53636j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7029868--7029871.cif.'
_cod_original_cell_volume        3520.0(2)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C28 H32 MN2 N20'
_cod_database_code               7029870
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 193,X'S) H   ( 191,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = N(21) TO N(22) 
U(IJ)'S  0.0, 0.010000 = N(24) TO N(25) 
END                                                                             
;
#END Tags that were not found in dictionaries
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
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mn1 Mn 0.28139(2) 0.234370(12) 0.411321(12) 0.0350 1.0000 Uani . .
N1 N 0.26540(12) 0.31879(7) 0.32063(7) 0.0396 1.0000 Uani . .
C3 C 0.17233(15) 0.31715(11) 0.26521(9) 0.0484 1.0000 Uani . .
C4 C 0.15931(19) 0.37108(13) 0.21404(11) 0.0622 1.0000 Uani . .
C5 C 0.2440(2) 0.42809(13) 0.21960(13) 0.0701 1.0000 Uani . .
C6 C 0.33856(19) 0.43155(10) 0.27661(11) 0.0565 1.0000 Uani . .
C7 C 0.34696(15) 0.37578(8) 0.32670(9) 0.0404 1.0000 Uani . .
C8 C 0.44749(16) 0.37731(8) 0.39027(9) 0.0433 1.0000 Uani . .
N3 N 0.48748(12) 0.30339(7) 0.41227(7) 0.0362 1.0000 Uani . .
C10 C 0.55839(16) 0.30243(11) 0.48485(9) 0.0482 1.0000 Uani . .
C11 C 0.67753(19) 0.34812(13) 0.49067(10) 0.0585 1.0000 Uani . .
C12 C 0.7698(2) 0.38535(16) 0.49239(14) 0.0803 1.0000 Uani . .
C13 C 0.56653(14) 0.26914(9) 0.35974(8) 0.0399 1.0000 Uani . .
C14 C 0.54123(15) 0.18932(8) 0.35806(8) 0.0387 1.0000 Uani . .
N2 N 0.43146(14) 0.16121(7) 0.37673(8) 0.0445 1.0000 Uani . .
C16 C 0.4436(2) 0.08756(10) 0.36983(11) 0.0542 1.0000 Uani . .
C17 C 0.5587(2) 0.07132(10) 0.34533(11) 0.0580 1.0000 Uani . .
N18 N 0.62145(15) 0.13681(8) 0.33790(8) 0.0490 1.0000 Uani . .
C19 C 0.7520(2) 0.14531(14) 0.31475(14) 0.0707 1.0000 Uani . .
N12 N 0.19694(15) 0.31616(7) 0.47973(7) 0.0455 1.0000 Uani . .
N31 N 0.13496(15) 0.36789(8) 0.45876(8) 0.0472 1.0000 Uani . U
N32 N 0.0766(2) 0.41755(12) 0.43809(12) 0.0853 1.0000 Uani . U
N9 N 0.11322(15) 0.17959(9) 0.36186(9) 0.0580 1.0000 Uani . .
N34 N 0.09380(15) 0.11772(10) 0.35644(11) 0.0624 1.0000 Uani . U
N35 N 0.0719(3) 0.05739(14) 0.3500(2) 0.1292 1.0000 Uani . U
H31 H 0.1135 0.2757 0.2623 0.0596 1.0000 Uiso R .
H41 H 0.0908 0.3673 0.1744 0.0766 1.0000 Uiso R .
H51 H 0.2393 0.4665 0.1842 0.0844 1.0000 Uiso R .
H61 H 0.3972 0.4734 0.2808 0.0704 1.0000 Uiso R .
H82 H 0.4094 0.4009 0.4313 0.0532 1.0000 Uiso R .
H81 H 0.5241 0.4059 0.3786 0.0533 1.0000 Uiso R .
H102 H 0.4981 0.3209 0.5194 0.0591 1.0000 Uiso R .
H101 H 0.5833 0.2505 0.4973 0.0600 1.0000 Uiso R .
H121 H 0.8466 0.4171 0.4936 0.0964 1.0000 Uiso R .
H131 H 0.6609 0.2797 0.3717 0.0493 1.0000 Uiso R .
H132 H 0.5411 0.2907 0.3114 0.0490 1.0000 Uiso R .
H161 H 0.3765 0.0525 0.3817 0.0669 1.0000 Uiso R .
H171 H 0.5945 0.0245 0.3352 0.0726 1.0000 Uiso R .
H192 H 0.7976 0.1000 0.3216 0.1105 1.0000 Uiso R .
H193 H 0.7981 0.1840 0.3446 0.1097 1.0000 Uiso R .
H191 H 0.7448 0.1601 0.2642 0.1099 1.0000 Uiso R .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N12 4_556 Mn1 N1 . 161.98(5) yes
N12 4_556 Mn1 N3 . 101.55(5) yes
N1 . Mn1 N3 . 69.79(4) yes
N12 4_556 Mn1 N2 . 90.08(5) yes
N1 . Mn1 N2 . 101.64(6) yes
N3 . Mn1 N2 . 72.19(5) yes
N12 4_556 Mn1 N12 . 76.53(5) yes
N1 . Mn1 N12 . 87.71(5) yes
N3 . Mn1 N12 . 91.56(5) yes
N2 . Mn1 N12 . 156.63(5) yes
N12 4_556 Mn1 N9 . 101.66(7) yes
N1 . Mn1 N9 . 90.28(6) yes
N3 . Mn1 N9 . 154.83(6) yes
N2 . Mn1 N9 . 98.16(7) yes
N12 . Mn1 N9 . 103.22(7) yes
Mn1 . N1 C3 . 123.37(12) yes
Mn1 . N1 C7 . 118.05(10) yes
C3 . N1 C7 . 118.35(15) yes
N1 . C3 C4 . 122.29(18) yes
N1 . C3 H31 . 117.0 no
C4 . C3 H31 . 120.7 no
C3 . C4 C5 . 119.15(18) yes
C3 . C4 H41 . 119.4 no
C5 . C4 H41 . 121.4 no
C4 . C5 C6 . 119.55(18) yes
C4 . C5 H51 . 121.6 no
C6 . C5 H51 . 118.8 no
C5 . C6 C7 . 118.8(2) yes
C5 . C6 H61 . 118.9 no
C7 . C6 H61 . 122.3 no
C6 . C7 N1 . 121.79(17) yes
C6 . C7 C8 . 120.95(16) yes
N1 . C7 C8 . 117.26(13) yes
C7 . C8 N3 . 110.88(12) yes
C7 . C8 H82 . 109.2 no
N3 . C8 H82 . 108.0 no
C7 . C8 H81 . 109.6 no
N3 . C8 H81 . 110.5 no
H82 . C8 H81 . 108.5 no
C8 . N3 Mn1 . 105.14(9) yes
C8 . N3 C10 . 111.54(13) yes
Mn1 . N3 C10 . 110.23(9) yes
C8 . N3 C13 . 111.56(12) yes
Mn1 . N3 C13 . 107.48(9) yes
C10 . N3 C13 . 110.67(12) yes
N3 . C10 C11 . 112.97(15) yes
N3 . C10 H102 . 108.0 no
C11 . C10 H102 . 108.5 no
N3 . C10 H101 . 108.3 no
C11 . C10 H101 . 109.5 no
H102 . C10 H101 . 109.5 no
C10 . C11 C12 . 177.1(2) yes
C11 . C12 H121 . 179.3 no
N3 . C13 C14 . 109.29(12) yes
N3 . C13 H131 . 110.7 no
C14 . C13 H131 . 111.3 no
N3 . C13 H132 . 108.6 no
C14 . C13 H132 . 110.1 no
H131 . C13 H132 . 106.8 no
C13 . C14 N2 . 122.24(13) yes
C13 . C14 N18 . 127.17(14) yes
N2 . C14 N18 . 110.59(14) yes
Mn1 . N2 C14 . 118.59(11) yes
Mn1 . N2 C16 . 135.27(12) yes
C14 . N2 C16 . 106.13(15) yes
N2 . C16 C17 . 110.12(17) yes
N2 . C16 H161 . 123.9 no
C17 . C16 H161 . 126.0 no
C16 . C17 N18 . 105.84(16) yes
C16 . C17 H171 . 129.1 no
N18 . C17 H171 . 125.0 no
C17 . N18 C14 . 107.30(15) yes
C17 . N18 C19 . 125.08(17) yes
C14 . N18 C19 . 127.59(17) yes
N18 . C19 H192 . 108.5 no
N18 . C19 H193 . 108.1 no
H192 . C19 H193 . 110.6 no
N18 . C19 H191 . 109.4 no
H192 . C19 H191 . 111.1 no
H193 . C19 H191 . 109.1 no
Mn1 . N12 Mn1 4_556 103.47(6) yes
Mn1 . N12 N31 . 125.70(12) yes
Mn1 4_556 N12 N31 . 129.60(12) yes
N12 . N31 N32 . 179.21(19) yes
Mn1 . N9 N34 . 128.95(15) yes
N9 . N34 N35 . 178.3(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 N12 4_556 2.2307(14) yes
Mn1 N1 . 2.2960(14) yes
Mn1 N3 . 2.4664(15) yes
Mn1 N2 . 2.1916(15) yes
Mn1 N12 . 2.2088(14) yes
Mn1 N9 . 2.1310(16) yes
N1 C3 . 1.339(2) yes
N1 C7 . 1.342(2) yes
C3 C4 . 1.378(3) yes
C3 H31 . 0.972 no
C4 C5 . 1.362(3) yes
C4 H41 . 0.974 no
C5 C6 . 1.371(3) yes
C5 H51 . 0.969 no
C6 C7 . 1.388(2) yes
C6 H61 . 0.977 no
C7 C8 . 1.496(2) yes
C8 N3 . 1.471(2) yes
C8 H82 . 0.994 no
C8 H81 . 0.989 no
N3 C10 . 1.476(2) yes
N3 C13 . 1.4751(19) yes
C10 C11 . 1.480(3) yes
C10 H102 . 0.997 no
C10 H101 . 1.013 no
C11 C12 . 1.168(3) yes
C12 H121 . 0.980 no
C13 C14 . 1.495(2) yes
C13 H131 . 0.991 no
C13 H132 . 0.998 no
C14 N2 . 1.317(2) yes
C14 N18 . 1.348(2) yes
N2 C16 . 1.372(2) yes
C16 C17 . 1.342(3) yes
C16 H161 . 0.986 no
C17 N18 . 1.382(3) yes
C17 H171 . 0.965 no
N18 C19 . 1.455(3) yes
C19 H192 . 0.960 no
C19 H193 . 0.997 no
C19 H191 . 0.979 no
N12 N31 . 1.1917(19) yes
N31 N32 . 1.141(2) yes
N9 N34 . 1.161(2) yes
N34 N35 . 1.140(3) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C3 H31 N9 . 123.10 0.972 2.571 3.207(3) yes
C10 H102 N9 4_556 154.88 0.997 2.593 3.521(3) yes
