#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:07:20 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178935 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/64/4116450.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_4116450
loop_
_publ_author_name
'F. Albert Cotton'
'Lee M. Daniels'
'Carlos A. Murillo'
'Isabel Pascual'
'Hong-Cai Zhou'
_publ_section_title
;
 Remarkable Effects of Axial π* Coordination on the Cr-Cr Quadruple Bond
 in Dichromium Paddlewheel Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6856
_journal_page_last               6861
_journal_paper_doi               10.1021/ja9912675
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_moiety         'Cr2 (C10 H8 N3)4, 2(C H2 Cl2)'
_chemical_formula_structural     'Cr2 (dpa)4, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl4 Cr2 N12'
_chemical_formula_weight         954.63
_chemical_name_systematic
; 
 Tetrakis(2,2'-dipyridylamidinato)dichromium(II) 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.763(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.966(6)
_cell_length_b                   9.581(2)
_cell_length_c                   19.106(4)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      9.0
_cell_volume                     4242.3(16)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    XPW
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8063
_diffrn_reflns_theta_max         22.53
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        none
_diffrn_standards_number         'none (area detector)'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'bright red'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    none
_exptl_crystal_description       'truncated pyramid'
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_obs          0.0510
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0618P)²+19.9819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1319
_refine_ls_wR_factor_obs         0.1255
_reflns_number_observed          2449
_reflns_number_total             2718
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9912675_1.cif
_cod_data_source_block           3.2CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+19.9819P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+19.9819P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4242.3(17)
_cod_database_code               4116450
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cr1 Cr -0.46441(2) -0.39351(6) 0.23464(3) 0.0233(2) Uani 1 d .
N1 N -0.57785(13) -0.2497(3) 0.1890(2) 0.0258(7) Uani 1 d .
N2 N -0.49057(13) -0.2314(3) 0.16436(15) 0.0265(7) Uani 1 d .
N3 N -0.40167(14) -0.2594(3) 0.1476(2) 0.0356(8) Uani 1 d .
N10 N -0.50733(13) -0.5369(3) 0.3471(2) 0.0268(7) Uani 1 d .
N20 N -0.42889(13) -0.5545(3) 0.3016(2) 0.0287(7) Uani 1 d .
N30 N -0.3485(2) -0.5360(4) 0.2595(2) 0.0439(9) Uani 1 d .
C1 C -0.6342(2) -0.2169(4) 0.1773(2) 0.0343(10) Uani 1 d .
H1 H -0.6509(16) -0.2610(39) 0.2031(20) 0.022(10) Uiso 1 d .
C2 C -0.6616(2) -0.1228(4) 0.1265(2) 0.0395(10) Uani 1 d .
H2 H -0.7013(22) -0.1034(45) 0.1204(25) 0.050(13) Uiso 1 d .
C3 C -0.6303(2) -0.0619(5) 0.0831(2) 0.0404(10) Uani 1 d .
H3 H -0.6467(19) -0.0075(46) 0.0484(25) 0.043(12) Uiso 1 d .
C4 C -0.5732(2) -0.0926(4) 0.0927(2) 0.0341(10) Uani 1 d .
H4 H -0.5542(18) -0.0556(43) 0.0612(23) 0.037(11) Uiso 1 d .
C5 C -0.5459(2) -0.1866(4) 0.1481(2) 0.0273(9) Uani 1 d .
C6 C -0.4459(2) -0.1701(4) 0.1425(2) 0.0283(9) Uani 1 d .
C7 C -0.4413(2) -0.0308(5) 0.1236(2) 0.0373(10) Uani 1 d .
H7 H -0.4685(18) 0.0257(44) 0.1247(21) 0.033(11) Uiso 1 d .
C8 C -0.3919(2) 0.0132(6) 0.1066(2) 0.0490(12) Uani 1 d .
H8 H -0.3876(23) 0.1012(57) 0.0959(29) 0.066(16) Uiso 1 d .
C9 C -0.3475(2) -0.0791(6) 0.1097(2) 0.0526(13) Uani 1 d .
H9 H -0.3146(22) -0.0513(51) 0.0987(26) 0.056(14) Uiso 1 d .
C10 C -0.3544(2) -0.2120(6) 0.1309(2) 0.0471(12) Uani 1 d .
H10 H -0.3284(20) -0.2763(47) 0.1331(23) 0.042(13) Uiso 1 d .
C11 C -0.5370(2) -0.5687(4) 0.3971(2) 0.0330(9) Uani 1 d .
H11 H -0.5703(19) -0.5236(45) 0.3922(22) 0.040 Uiso 1 d .
C12 C -0.5178(2) -0.6626(4) 0.4513(2) 0.0389(10) Uani 1 d .
H12 H -0.5390(19) -0.6825(47) 0.4823(25) 0.047(13) Uiso 1 d .
C13 C -0.4651(2) -0.7280(4) 0.4566(2) 0.0378(10) Uani 1 d .
H13 H -0.4506(18) -0.7888(44) 0.4932(23) 0.038(11) Uiso 1 d .
C14 C -0.4342(2) -0.6989(4) 0.4072(2) 0.0341(9) Uani 1 d .
H14 H -0.3967(18) -0.7394(41) 0.4139(21) 0.034(11) Uiso 1 d .
C15 C -0.4558(2) -0.6016(4) 0.3514(2) 0.0277(9) Uani 1 d .
C16 C -0.3829(2) -0.6224(4) 0.2842(2) 0.0297(9) Uani 1 d .
C17 C -0.3743(2) -0.7668(4) 0.2860(2) 0.0394(10) Uani 1 d .
H17 H -0.4004(21) -0.8241(50) 0.3005(25) 0.052(13) Uiso 1 d .
C18 C -0.3284(2) -0.8202(5) 0.2634(2) 0.0481(12) Uani 1 d .
H18 H -0.3219(20) -0.9149(52) 0.2631(25) 0.052(13) Uiso 1 d .
C19 C -0.2921(2) -0.7316(5) 0.2402(3) 0.0522(13) Uani 1 d .
H19 H -0.2629(22) -0.7620(51) 0.2251(25) 0.055(14) Uiso 1 d .
C20 C -0.3045(2) -0.5931(5) 0.2380(3) 0.0546(13) Uani 1 d .
H20 H -0.2831(21) -0.5249(53) 0.2230(26) 0.059(14) Uiso 1 d .
C99 C -0.1800(4) 0.0524(8) 0.0324(4) 0.163(5) Uani 1 d .
H99A H -0.1409(4) 0.0287(8) 0.0604(4) 0.195 Uiso 1 calc R
H99B H -0.1965(4) 0.1164(8) 0.0618(4) 0.195 Uiso 1 calc R
Cl1 Cl -0.21958(8) -0.0936(2) 0.01906(12) 0.1013(6) Uani 1 d .
Cl2 Cl -0.17496(8) 0.1408(2) -0.04652(11) 0.1075(7) Uani 1 d .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
Cr1 Cr1 N2 93.02(9) 6_456 .
Cr1 Cr1 N20 93.94(9) 6_456 .
N2 Cr1 N20 173.03(12) . .
Cr1 Cr1 N10 94.87(9) 6_456 6_456
N2 Cr1 N10 91.26(12) . 6_456
N20 Cr1 N10 88.58(12) . 6_456
Cr1 Cr1 N1 95.53(8) 6_456 6_456
N2 Cr1 N1 88.33(12) . 6_456
N20 Cr1 N1 90.57(12) . 6_456
N10 Cr1 N1 169.60(11) 6_456 6_456
C1 N1 C5 119.0(3) . .
C1 N1 Cr1 124.1(3) . 6_456
C5 N1 Cr1 116.9(2) . 6_456
C5 N2 C6 125.9(3) . .
C5 N2 Cr1 120.7(2) . .
C6 N2 Cr1 113.1(2) . .
C10 N3 C6 117.8(4) . .
C11 N10 C15 118.8(3) . .
C11 N10 Cr1 123.5(3) . 6_456
C15 N10 Cr1 117.8(2) . 6_456
C15 N20 C16 124.0(3) . .
C15 N20 Cr1 119.6(2) . .
C16 N20 Cr1 115.6(2) . .
C16 N30 C20 117.3(4) . .
N1 C1 C2 123.6(4) . .
N1 C1 H1 113.5(26) . .
C2 C1 H1 122.8(26) . .
C1 C2 C3 117.9(4) . .
C1 C2 H2 120.4(28) . .
C3 C2 H2 121.7(28) . .
C4 C3 C2 120.5(4) . .
C4 C3 H3 118.8(29) . .
C2 C3 H3 120.6(29) . .
C3 C4 C5 119.7(4) . .
C3 C4 H4 118.6(26) . .
C5 C4 H4 121.6(26) . .
N2 C5 N1 112.8(3) . .
N2 C5 C4 127.9(3) . .
N1 C5 C4 119.2(3) . .
N3 C6 N2 111.4(3) . .
N3 C6 C7 121.0(4) . .
N2 C6 C7 127.4(4) . .
C8 C7 C6 119.1(4) . .
C8 C7 H7 121.5(28) . .
C6 C7 H7 119.3(27) . .
C9 C8 C7 119.8(5) . .
C9 C8 H8 119.6(35) . .
C7 C8 H8 120.5(36) . .
C10 C9 C8 117.8(4) . .
C10 C9 H9 121.5(32) . .
C8 C9 H9 120.7(32) . .
N3 C10 C9 124.5(5) . .
N3 C10 H10 112.9(29) . .
C9 C10 H10 122.6(29) . .
C12 C11 N10 123.2(4) . .
C12 C11 H11 121.3(27) . .
N10 C11 H11 115.5(27) . .
C11 C12 C13 118.5(4) . .
C11 C12 H12 120.5(29) . .
C13 C12 H12 121.0(29) . .
C14 C13 C12 120.0(4) . .
C14 C13 H13 119.5(26) . .
C12 C13 H13 120.5(26) . .
C13 C14 C15 119.7(4) . .
C13 C14 H14 118.8(23) . .
C15 C14 H14 121.3(24) . .
N20 C15 N10 113.0(3) . .
N20 C15 C14 127.0(4) . .
N10 C15 C14 119.8(3) . .
N30 C16 N20 113.1(3) . .
N30 C16 C17 121.4(4) . .
N20 C16 C17 125.3(4) . .
C18 C17 C16 118.9(4) . .
C18 C17 H17 121.9(29) . .
C16 C17 H17 119.1(29) . .
C19 C18 C17 119.7(4) . .
C19 C18 H18 119.1(29) . .
C17 C18 H18 121.2(29) . .
C20 C19 C18 117.6(4) . .
C20 C19 H19 120.3(33) . .
C18 C19 H19 122.0(33) . .
N30 C20 C19 124.9(5) . .
N30 C20 H20 110.4(30) . .
C19 C20 H20 124.7(30) . .
Cl1 C99 Cl2 115.6(4) . .
Cl1 C99 H99A 108.4(3) . .
Cl2 C99 H99A 108.4(3) . .
Cl1 C99 H99B 108.4(4) . .
Cl2 C99 H99B 108.4(3) . .
H99A C99 H99B 107.4 . .
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
Cr1 Cr1 1.9404(11) 6_456 y
Cr1 N2 2.044(3) . y
Cr1 N20 2.046(3) . y
Cr1 N1 2.074(3) 6_456 y
N1 C1 1.348(5) . ?
N1 C5 1.367(5) . ?
N1 Cr1 2.074(3) 6_456 ?
N2 C5 1.352(5) . ?
N2 C6 1.377(5) . ?
N3 C10 1.333(6) . ?
N3 C6 1.347(5) . ?
N10 C11 1.362(5) . ?
N10 C15 1.366(5) . ?
N10 Cr1 2.060(3) 6_456 ?
N20 C15 1.356(5) . ?
N20 C16 1.391(5) . ?
N30 C16 1.336(5) . ?
N30 C20 1.342(6) . ?
C1 C2 1.365(6) . ?
C1 H1 0.83(4) . ?
C2 C3 1.381(6) . ?
C2 H2 0.95(5) . ?
C3 C4 1.366(6) . ?
C3 H3 0.86(5) . ?
C4 C5 1.416(6) . ?
C4 H4 0.91(4) . ?
C6 C7 1.394(6) . ?
C7 C8 1.372(6) . ?
C7 H7 0.85(4) . ?
C8 C9 1.372(7) . ?
C8 H8 0.88(5) . ?
C9 C10 1.359(7) . ?
C9 H9 0.91(5) . ?
C10 H10 0.87(5) . ?
C11 C12 1.360(6) . ?
C11 H11 0.89(4) . ?
C12 C13 1.390(6) . ?
C12 H12 0.89(5) . ?
C13 C14 1.369(6) . ?
C13 H13 0.91(4) . ?
C14 C15 1.412(5) . ?
C14 H14 0.96(4) . ?
C16 C17 1.398(6) . ?
C17 C18 1.378(6) . ?
C17 H17 0.93(5) . ?
C18 C19 1.368(7) . ?
C18 H18 0.92(5) . ?
C19 C20 1.358(7) . ?
C19 H19 0.87(5) . ?
C20 H20 0.92(5) . ?
C99 Cl1 1.673(9) . ?
C99 Cl2 1.760(10) . ?
C99 H99A 0.98 . ?
C99 H99B 0.98 . ?
