#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:04:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179091 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305316.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_4305316
loop_
_publ_author_name
'Meenakshi Ghosh'
'Stephen Sproules'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
(α-Diimine)chromium Complexes: Molecular and Electronic Structures; A
Combined Experimental and Density Functional Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5963
_journal_page_last               5970
_journal_paper_doi               10.1021/ic800290s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C38 H54 Cr N2 O4'
_chemical_formula_weight         654.83
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.743(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.835(2)
_cell_length_b                   12.5567(10)
_cell_length_c                   27.350(2)
_cell_measurement_temperature    100(2)
_cell_volume                     7498.1(11)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
"'2833 images at 0.3 deg. stepwise rotation in omega and phi, 36 sec./frame"
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55245
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8229
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0562
_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)+(0.0305P)²+12.6930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                6022
_reflns_number_total             8549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800290s-file001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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_database_code               4305316
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_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
Cr1 Cr 0.359017(15) 0.88274(3) 0.598281(12) 0.01902(9) Uani 1 1 d . . .
N1 N 0.33380(8) 1.01108(14) 0.63602(6) 0.0202(4) Uani 1 1 d . . .
C2 C 0.32144(9) 0.98909(17) 0.68331(8) 0.0230(5) Uani 1 1 d . . .
C3 C 0.30983(9) 0.88003(18) 0.69327(8) 0.0227(4) Uani 1 1 d . . .
N4 N 0.31536(8) 0.81368(14) 0.65443(6) 0.0201(4) Uani 1 1 d . . .
C5 C 0.28728(10) 0.70981(17) 0.65514(8) 0.0220(5) Uani 1 1 d . . .
C6 C 0.32277(10) 0.61763(18) 0.66407(7) 0.0241(4) Uani 1 1 d . . .
C7 C 0.29368(11) 0.51825(18) 0.66066(8) 0.0280(5) Uani 1 1 d . . .
H7 H 0.3169 0.4552 0.6661 0.034 Uiso 1 1 calc R . .
C8 C 0.23161(11) 0.51027(19) 0.64944(8) 0.0309(5) Uani 1 1 d . . .
H8 H 0.2129 0.4422 0.6466 0.037 Uiso 1 1 calc R . .
C9 C 0.19704(11) 0.60136(19) 0.64233(8) 0.0299(5) Uani 1 1 d . . .
H9 H 0.1545 0.5950 0.6354 0.036 Uiso 1 1 calc R . .
C10 C 0.22354(10) 0.70270(18) 0.64522(8) 0.0260(5) Uani 1 1 d . . .
C11 C 0.33554(9) 1.11952(17) 0.61836(7) 0.0217(4) Uani 1 1 d . . .
C12 C 0.28185(10) 1.16293(17) 0.59674(8) 0.0232(5) Uani 1 1 d . . .
C13 C 0.28511(11) 1.26509(18) 0.57626(8) 0.0296(5) Uani 1 1 d . . .
H13 H 0.2495 1.2956 0.5617 0.035 Uiso 1 1 calc R . .
C14 C 0.33947(12) 1.32253(18) 0.57688(9) 0.0319(5) Uani 1 1 d . . .
H14 H 0.3411 1.3912 0.5623 0.038 Uiso 1 1 calc R . .
C15 C 0.39126(11) 1.27936(18) 0.59875(8) 0.0299(5) Uani 1 1 d . . .
H15 H 0.4282 1.3194 0.5992 0.036 Uiso 1 1 calc R . .
C16 C 0.39064(10) 1.17787(17) 0.62030(8) 0.0245(5) Uani 1 1 d . . .
C17 C 0.31963(11) 1.07258(18) 0.72290(8) 0.0304(5) Uani 1 1 d . . .
H17A H 0.3561 1.0659 0.7440 0.046 Uiso 1 1 calc R . .
H17B H 0.2828 1.0626 0.7425 0.046 Uiso 1 1 calc R . .
H17C H 0.3188 1.1435 0.7080 0.046 Uiso 1 1 calc R . .
C18 C 0.29027(11) 0.84420(19) 0.74305(8) 0.0297(5) Uani 1 1 d . . .
H18A H 0.2773 0.7696 0.7415 0.044 Uiso 1 1 calc R . .
H18B H 0.2561 0.8884 0.7540 0.044 Uiso 1 1 calc R . .
H18C H 0.3247 0.8513 0.7662 0.044 Uiso 1 1 calc R . .
C19 C 0.39015(10) 0.62405(18) 0.67910(8) 0.0282(5) Uani 1 1 d . . .
H19 H 0.4060 0.6950 0.6685 0.034 Uiso 1 1 calc R . .
C20 C 0.42982(11) 0.5383(2) 0.65560(10) 0.0372(6) Uani 1 1 d . . .
H20A H 0.4201 0.4688 0.6698 0.056 Uiso 1 1 calc R . .
H20B H 0.4732 0.5546 0.6616 0.056 Uiso 1 1 calc R . .
H20C H 0.4217 0.5366 0.6203 0.056 Uiso 1 1 calc R . .
C21 C 0.39728(12) 0.6174(2) 0.73551(9) 0.0435(6) Uani 1 1 d . . .
H21A H 0.3747 0.6761 0.7506 0.065 Uiso 1 1 calc R . .
H21B H 0.4407 0.6228 0.7446 0.065 Uiso 1 1 calc R . .
H21C H 0.3809 0.5493 0.7470 0.065 Uiso 1 1 calc R . .
C22 C 0.18330(11) 0.8007(2) 0.63815(9) 0.0335(6) Uani 1 1 d . . .
H22 H 0.2108 0.8644 0.6369 0.040 Uiso 1 1 calc R . .
C23 C 0.14020(12) 0.8151(2) 0.68201(11) 0.0459(7) Uani 1 1 d . . .
H23A H 0.1123 0.7541 0.6838 0.069 Uiso 1 1 calc R . .
H23B H 0.1164 0.8806 0.6777 0.069 Uiso 1 1 calc R . .
H23C H 0.1646 0.8196 0.7123 0.069 Uiso 1 1 calc R . .
C24 C 0.14631(11) 0.7968(2) 0.59014(10) 0.0427(7) Uani 1 1 d . . .
H24A H 0.1741 0.7849 0.5628 0.064 Uiso 1 1 calc R . .
H24B H 0.1247 0.8644 0.5854 0.064 Uiso 1 1 calc R . .
H24C H 0.1165 0.7385 0.5915 0.064 Uiso 1 1 calc R . .
C25 C 0.22110(10) 1.10298(19) 0.59735(8) 0.0267(5) Uani 1 1 d . . .
H25 H 0.2307 1.0251 0.5972 0.032 Uiso 1 1 calc R . .
C26 C 0.18005(11) 1.1256(2) 0.55266(9) 0.0371(6) Uani 1 1 d . . .
H26A H 0.1645 1.1987 0.5544 0.056 Uiso 1 1 calc R . .
H26B H 0.1455 1.0757 0.5522 0.056 Uiso 1 1 calc R . .
H26C H 0.2038 1.1168 0.5228 0.056 Uiso 1 1 calc R . .
C27 C 0.18589(11) 1.1266(2) 0.64449(9) 0.0409(6) Uani 1 1 d . . .
H27A H 0.2106 1.1044 0.6729 0.061 Uiso 1 1 calc R . .
H27B H 0.1471 1.0874 0.6440 0.061 Uiso 1 1 calc R . .
H27C H 0.1776 1.2032 0.6466 0.061 Uiso 1 1 calc R . .
C28 C 0.44834(10) 1.13708(19) 0.64607(9) 0.0295(5) Uani 1 1 d . . .
H28 H 0.4389 1.0658 0.6605 0.035 Uiso 1 1 calc R . .
C29 C 0.50165(10) 1.1231(2) 0.61054(10) 0.0370(6) Uani 1 1 d . . .
H29A H 0.4907 1.0693 0.5860 0.055 Uiso 1 1 calc R . .
H29B H 0.5383 1.1000 0.6287 0.055 Uiso 1 1 calc R . .
H29C H 0.5099 1.1910 0.5943 0.055 Uiso 1 1 calc R . .
C30 C 0.46761(12) 1.2122(2) 0.68817(10) 0.0420(7) Uani 1 1 d . . .
H30A H 0.5021 1.1808 0.7064 0.063 Uiso 1 1 calc R . .
H30B H 0.4330 1.2224 0.7102 0.063 Uiso 1 1 calc R . .
H30C H 0.4799 1.2812 0.6747 0.063 Uiso 1 1 calc R . .
O31 O 0.28801(6) 0.87661(12) 0.55253(5) 0.0211(3) Uani 1 1 d . . .
C32 C 0.28309(10) 0.91861(17) 0.50964(8) 0.0226(5) Uani 1 1 d . . .
C33 C 0.32688(10) 0.98531(18) 0.48875(8) 0.0258(5) Uani 1 1 d . . .
H33 H 0.3174 1.0159 0.4578 0.031 Uiso 1 1 calc R . .
C34 C 0.38351(10) 1.01017(17) 0.51003(8) 0.0234(5) Uani 1 1 d . . .
O35 O 0.40401(6) 0.97141(12) 0.55048(5) 0.0234(3) Uani 1 1 d . . .
C36 C 0.42461(11) 1.08968(19) 0.48479(9) 0.0303(5) Uani 1 1 d . . .
H36A H 0.4247 1.1569 0.5030 0.045 Uiso 1 1 calc R . .
H36B H 0.4094 1.1022 0.4514 0.045 Uiso 1 1 calc R . .
H36C H 0.4664 1.0614 0.4836 0.045 Uiso 1 1 calc R . .
C37 C 0.22536(10) 0.89293(19) 0.48082(8) 0.0273(5) Uani 1 1 d . . .
H37A H 0.2239 0.8163 0.4740 0.041 Uiso 1 1 calc R . .
H37B H 0.2253 0.9325 0.4499 0.041 Uiso 1 1 calc R . .
H37C H 0.1895 0.9134 0.4999 0.041 Uiso 1 1 calc R . .
O41 O 0.43589(6) 0.88046(12) 0.63925(5) 0.0230(3) Uani 1 1 d . . .
C42 C 0.48563(10) 0.83039(18) 0.63068(8) 0.0262(5) Uani 1 1 d . . .
C43 C 0.49325(10) 0.75653(18) 0.59291(9) 0.0282(5) Uani 1 1 d . . .
H43 H 0.5331 0.7288 0.5877 0.034 Uiso 1 1 calc R . .
C44 C 0.44550(10) 0.72102(18) 0.56225(8) 0.0269(5) Uani 1 1 d . . .
O45 O 0.38996(7) 0.75234(12) 0.56421(5) 0.0245(3) Uani 1 1 d . . .
C46 C 0.45886(12) 0.6378(2) 0.52351(10) 0.0397(6) Uani 1 1 d . . .
H46A H 0.4281 0.5810 0.5250 0.060 Uiso 1 1 calc R . .
H46B H 0.4997 0.6076 0.5294 0.060 Uiso 1 1 calc R . .
H46C H 0.4574 0.6710 0.4911 0.060 Uiso 1 1 calc R . .
C47 C 0.53832(11) 0.8525(2) 0.66602(10) 0.0369(6) Uani 1 1 d . . .
H47A H 0.5411 0.9292 0.6722 0.055 Uiso 1 1 calc R . .
H47B H 0.5767 0.8274 0.6518 0.055 Uiso 1 1 calc R . .
H47C H 0.5312 0.8150 0.6969 0.055 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'
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
_geom_angle_publ_flag
O31 Cr1 O35 89.75(6) . . ?
O31 Cr1 N1 98.00(6) . . ?
O35 Cr1 N1 91.71(7) . . ?
O31 Cr1 O45 86.58(6) . . ?
O35 Cr1 O45 88.82(6) . . ?
N1 Cr1 O45 175.39(7) . . ?
O31 Cr1 O41 173.93(6) . . ?
O35 Cr1 O41 87.61(6) . . ?
N1 Cr1 O41 87.54(7) . . ?
O45 Cr1 O41 87.90(6) . . ?
O31 Cr1 N4 95.20(6) . . ?
O35 Cr1 N4 170.37(7) . . ?
N1 Cr1 N4 79.44(7) . . ?
O45 Cr1 N4 99.70(7) . . ?
O41 Cr1 N4 88.21(6) . . ?
C2 N1 C11 121.19(17) . . ?
C2 N1 Cr1 112.92(14) . . ?
C11 N1 Cr1 125.42(13) . . ?
N1 C2 C3 114.74(19) . . ?
N1 C2 C17 123.50(19) . . ?
C3 C2 C17 121.76(19) . . ?
N4 C3 C2 115.10(18) . . ?
N4 C3 C18 123.7(2) . . ?
C2 C3 C18 121.11(19) . . ?
C3 N4 C5 120.19(17) . . ?
C3 N4 Cr1 112.37(14) . . ?
C5 N4 Cr1 127.26(13) . . ?
C6 C5 C10 121.1(2) . . ?
C6 C5 N4 120.74(19) . . ?
C10 C5 N4 118.12(19) . . ?
C7 C6 C5 118.1(2) . . ?
C7 C6 C19 120.0(2) . . ?
C5 C6 C19 121.9(2) . . ?
C8 C7 C6 121.2(2) . . ?
C9 C8 C7 120.0(2) . . ?
C8 C9 C10 121.3(2) . . ?
C9 C10 C5 118.2(2) . . ?
C9 C10 C22 119.4(2) . . ?
C5 C10 C22 122.5(2) . . ?
C16 C11 C12 121.2(2) . . ?
C16 C11 N1 120.23(19) . . ?
C12 C11 N1 118.51(18) . . ?
C13 C12 C11 118.2(2) . . ?
C13 C12 C25 120.3(2) . . ?
C11 C12 C25 121.39(19) . . ?
C14 C13 C12 121.2(2) . . ?
C15 C14 C13 119.7(2) . . ?
C14 C15 C16 121.7(2) . . ?
C15 C16 C11 118.0(2) . . ?
C15 C16 C28 119.1(2) . . ?
C11 C16 C28 122.87(19) . . ?
C6 C19 C20 113.6(2) . . ?
C6 C19 C21 110.46(18) . . ?
C20 C19 C21 109.3(2) . . ?
C10 C22 C24 112.3(2) . . ?
C10 C22 C23 110.6(2) . . ?
C24 C22 C23 110.5(2) . . ?
C12 C25 C26 113.54(19) . . ?
C12 C25 C27 110.98(19) . . ?
C26 C25 C27 109.83(19) . . ?
C16 C28 C29 111.99(19) . . ?
C16 C28 C30 110.8(2) . . ?
C29 C28 C30 109.9(2) . . ?
C32 O31 Cr1 127.89(13) . . ?
O31 C32 C33 124.5(2) . . ?
O31 C32 C37 116.49(19) . . ?
C33 C32 C37 118.97(19) . . ?
C34 C33 C32 124.8(2) . . ?
O35 C34 C33 124.9(2) . . ?
O35 C34 C36 116.13(19) . . ?
C33 C34 C36 119.0(2) . . ?
C34 O35 Cr1 127.56(14) . . ?
C42 O41 Cr1 127.66(14) . . ?
O41 C42 C43 124.8(2) . . ?
O41 C42 C47 115.6(2) . . ?
C43 C42 C47 119.6(2) . . ?
C42 C43 C44 123.9(2) . . ?
O45 C44 C43 125.2(2) . . ?
O45 C44 C46 115.6(2) . . ?
C43 C44 C46 119.2(2) . . ?
C44 O45 Cr1 126.64(14) . . ?
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 O31 1.9813(14) . ?
Cr1 O35 1.9869(15) . ?
Cr1 N1 1.9950(17) . ?
Cr1 O45 2.0055(15) . ?
Cr1 O41 2.0063(14) . ?
Cr1 N4 2.0142(17) . ?
N1 C2 1.353(3) . ?
N1 C11 1.445(3) . ?
C2 C3 1.420(3) . ?
C2 C17 1.508(3) . ?
C3 N4 1.357(3) . ?
C3 C18 1.501(3) . ?
N4 C5 1.442(3) . ?
C5 C6 1.413(3) . ?
C5 C10 1.417(3) . ?
C6 C7 1.403(3) . ?
C6 C19 1.524(3) . ?
C7 C8 1.389(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.400(3) . ?
C10 C22 1.523(3) . ?
C11 C16 1.409(3) . ?
C11 C12 1.415(3) . ?
C12 C13 1.402(3) . ?
C12 C25 1.525(3) . ?
C13 C14 1.389(3) . ?
C14 C15 1.383(3) . ?
C15 C16 1.404(3) . ?
C16 C28 1.524(3) . ?
C19 C20 1.529(3) . ?
C19 C21 1.551(3) . ?
C22 C24 1.533(4) . ?
C22 C23 1.545(4) . ?
C25 C26 1.533(3) . ?
C25 C27 1.538(3) . ?
C28 C29 1.536(3) . ?
C28 C30 1.543(3) . ?
O31 C32 1.289(3) . ?
C32 C33 1.399(3) . ?
C32 C37 1.513(3) . ?
C33 C34 1.395(3) . ?
C34 O35 1.284(3) . ?
C34 C36 1.515(3) . ?
O41 C42 1.279(3) . ?
C42 C43 1.400(3) . ?
C42 C47 1.519(3) . ?
C43 C44 1.402(3) . ?
C44 O45 1.277(3) . ?
C44 C46 1.519(3) . ?
