#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:56:28 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143620 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/50/7035040.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_7035040
loop_
_publ_author_name
'Jeon, Jong Yeob'
'Park, Dong Sik'
'Lee, Dong Hwan'
'Eo, Seong Chan'
'Park, Seong Yeon'
'Jeong, Myoung Sun'
'Kang, Yi Young'
'Lee, Junseong'
'Lee, Bun Yeoul'
_publ_section_title
;
 A chromium precursor for the Phillips ethylene trimerization catalyst:
 (2-ethylhexanoate)2CrOH.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11004
_journal_page_last               11012
_journal_paper_doi               10.1039/c5dt01203a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C47 H68 Al2 Cr2 N6'
_chemical_formula_weight         875.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.396(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6000(3)
_cell_length_b                   12.6770(3)
_cell_length_c                   13.2740(2)
_cell_measurement_reflns_used    9503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.18
_cell_volume                     2331.26(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17283
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.436
_diffrn_reflns_theta_min         1.617
_exptl_absorpt_coefficient_mu    0.542
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0532P)²+2.0447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1718
_reflns_number_total             2261
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01203a2.cif
_cod_data_source_block           e:\frames\guest\lby\lby35\work\lby35-4
_cod_depositor_comments
'Adding full bibliography for 7035040--7035042.cif.'
_cod_database_code               7035040
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.958
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr 0.55410(4) 0.0000 0.68227(4) 0.0289(2) Uani 1 2 d S T P . .
N1 N 0.6079(2) 0.0000 0.5588(2) 0.0391(8) Uani 1 2 d S T P A .
N2 N 0.6303(5) 0.0840(5) 0.8476(5) 0.0237(16) Uani 0.5 1 d . . P A -1
N3 N 0.6579(3) 0.2216(3) 1.0380(3) 0.0294(10) Uani 0.5 1 d . . P A -1
Al Al 0.64676(10) 0.23219(11) 0.89095(11) 0.0287(3) Uani 0.5 1 d . . P A -1
C4 C 0.6948(2) 0(66) 0.8226(3) 0.0381(10) Uani 0.5 1 d . . P A -1
C5 C 0.6630(6) -0.0895(8) 0.8244(6) 0.0278(19) Uani 0.5 1 d . . P A -1
H5 H 0.6932 -0.1525 0.8123 0.033 Uiso 0.5 1 calc R U P A -1
C6 C 0.5771(6) -0.0850(6) 0.8467(5) 0.0237(15) Uani 0.5 1 d . . P A -1
H6 H 0.5386 -0.1436 0.8526 0.028 Uiso 0.5 1 calc R U P A -1
C7 C 0.5566(4) 0.0217(7) 0.8592(4) 0.025(3) Uani 0.5 1 d . . P A -1
C8 C 0.7862(3) 0.0483(4) 0.8019(4) 0.0338(12) Uani 0.5 1 d . . P A -1
H8A H 0.8334 0.0688 0.8697 0.051 Uiso 0.5 1 calc R U P A -1
H8B H 0.7673 0.1105 0.7562 0.051 Uiso 0.5 1 calc R U P A -1
H8C H 0.8150 -0.0043 0.7669 0.051 Uiso 0.5 1 calc R U P A -1
C9 C 0.4725(3) 0.0649(4) 0.8864(4) 0.0332(12) Uani 0.5 1 d . . P A -1
H9A H 0.4279 0.0074 0.8876 0.050 Uiso 0.5 1 calc R U P A -1
H9B H 0.4391 0.1171 0.8330 0.050 Uiso 0.5 1 calc R U P A -1
H9C H 0.4950 0.0985 0.9564 0.050 Uiso 0.5 1 calc R U P A -1
C10 C 0.7648(5) 0.2923(6) 0.8723(6) 0.0381(16) Uani 0.5 1 d . . P A -1
H10A H 0.7673 0.3682 0.8870 0.057 Uiso 0.5 1 calc R U P A -1
H10B H 0.7644 0.2807 0.7991 0.057 Uiso 0.5 1 calc R U P A -1
H10C H 0.8216 0.2580 0.9214 0.057 Uiso 0.5 1 calc R U P A -1
C11 C 0.5304(4) 0.3088(4) 0.8016(4) 0.0352(12) Uani 0.5 1 d . . P A -1
H11A H 0.4736 0.2848 0.8194 0.053 Uiso 0.5 1 calc R U P A -1
H11B H 0.5213 0.2946 0.7265 0.053 Uiso 0.5 1 calc R U P A -1
H11C H 0.5392 0.3847 0.8150 0.053 Uiso 0.5 1 calc R U P A -1
C12 C 0.7223(5) 0.1567(5) 1.1104(6) 0.0318(16) Uani 0.5 1 d . . P A -1
C13 C 0.7142(4) 0.1711(4) 1.2098(4) 0.0359(13) Uani 0.5 1 d . . P A -1
H13 H 0.7497 0.1356 1.2731 0.043 Uiso 0.5 1 calc R U P A -1
C14 C 0.6424(4) 0.2491(4) 1.1993(4) 0.0406(13) Uani 0.5 1 d . . P A -1
H14 H 0.6210 0.2760 1.2548 0.049 Uiso 0.5 1 calc R U P A -1
C15 C 0.6094(4) 0.2788(4) 1.0949(4) 0.0347(12) Uani 0.5 1 d . . P A -1
C16 C 0.7905(4) 0.0845(4) 1.0818(4) 0.0397(13) Uani 0.5 1 d . . P A -1
H16A H 0.8348 0.0533 1.1465 0.060 Uiso 0.5 1 calc R U P A -1
H16B H 0.8276 0.1242 1.0445 0.060 Uiso 0.5 1 calc R U P A -1
H16C H 0.7541 0.0283 1.0355 0.060 Uiso 0.5 1 calc R U P A -1
C17 C 0.5357(4) 0.3608(5) 1.0445(5) 0.0507(16) Uani 0.5 1 d . . P A -1
H17A H 0.5137 0.3948 1.0990 0.076 Uiso 0.5 1 calc R U P A -1
H17B H 0.4807 0.3276 0.9915 0.076 Uiso 0.5 1 calc R U P A -1
H17C H 0.5645 0.4138 1.0099 0.076 Uiso 0.5 1 calc R U P A -1
C57 C 1.1258(10) 0.027(3) 0.4476(15) 0.082(10) Uani 0.25 1 d D . P B -1
H57A H 1.1389 -0.0382 0.4148 0.122 Uiso 0.25 1 calc R U P B -1
H57B H 1.1816 0.0443 0.5092 0.122 Uiso 0.25 1 calc R U P B -1
H57C H 1.1138 0.0845 0.3960 0.122 Uiso 0.25 1 calc R U P B -1
C51 C 1.0355(5) 0.0109(19) 0.4841(7) 0.053(3) Uani 0.25 1 d DG U P B -1
C52 C 0.9485(6) -0.0119(13) 0.4066(6) 0.033(3) Uani 0.25 1 d G U P B -1
H52 H 0.9462 -0.0201 0.3347 0.039 Uiso 0.25 1 calc R U P B -1
C53 C 0.8647(5) -0.0228(18) 0.4343(8) 0.081(8) Uani 0.25 1 d G . P B -1
H53 H 0.8052 -0.0385 0.3813 0.097 Uiso 0.25 1 calc R U P B -1
C54 C 0.8680(7) -0.011(3) 0.5395(8) 0.081(11) Uani 0.25 1 d G U P B -1
H54 H 0.8108 -0.0184 0.5584 0.097 Uiso 0.25 1 calc R U P B -1
C55 C 0.9551(8) 0.012(3) 0.6170(6) 0.116(10) Uani 0.25 1 d G . P B -1
H55 H 0.9573 0.0201 0.6889 0.139 Uiso 0.25 1 calc R U P B -1
C56 C 1.0388(7) 0.023(3) 0.5893(6) 0.130(14) Uani 0.25 1 d G . P B -1
H56 H 1.0983 0.0385 0.6423 0.156 Uiso 0.25 1 calc R U P B -1
C1 C 0.6093(2) 0.0873(3) 0.4983(2) 0.0570(9) Uani 1 1 d . . . . .
C2 C 0.6067(2) 0.0558(3) 0.3974(2) 0.0786(15) Uani 1 1 d . . . . .
H2 H 0.6052 0.1005 0.3395 0.094 Uiso 1 1 calc R U . . .
C3 C 0.6193(3) 0.1957(3) 0.5442(3) 0.0878(15) Uani 1 1 d . . . . .
H3A H 0.6856 0.2061 0.5910 0.132 Uiso 1 1 calc R U . . .
H3B H 0.5744 0.2043 0.5852 0.132 Uiso 1 1 calc R U . . .
H3C H 0.6044 0.2478 0.4868 0.132 Uiso 1 1 calc R U . . .
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'
Al Al 0.0645 0.0514 '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
N1 Cr C4 100(10) . .
N1 Cr C5 108.27(19) . .
C4 Cr C5 31(10) . .
N1 Cr C7 156.67(18) . .
C4 Cr C7 58(10) . .
C5 Cr C7 57.3(2) . .
N1 Cr C2 102.82(10) . 5_656
C4 Cr C2 151(10) . 5_656
C5 Cr C2 122.9(2) . 5_656
C7 Cr C2 100.50(18) . 5_656
N1 Cr C2 102.82(10) . 2_656
C4 Cr C2 151(10) . 2_656
C5 Cr C2 146.4(2) . 2_656
C7 Cr C2 96.44(15) . 2_656
C2 Cr C2 34.9(2) 5_656 2_656
N1 Cr C6 140.2(2) . .
C4 Cr C6 55(10) . .
C5 Cr C6 34.1(2) . .
C7 Cr C6 34.7(3) . .
C2 Cr C6 96.3(2) 5_656 .
C2 Cr C6 112.5(2) 2_656 .
N1 Cr N2 123.94(18) . .
C4 Cr N2 38(10) . .
C5 Cr N2 58.15(19) . .
C7 Cr N2 34.0(2) . .
C2 Cr N2 131.16(19) 5_656 .
C2 Cr N2 112.9(2) 2_656 .
C6 Cr N2 57.5(2) . .
C1 N1 C1 107.6(3) . 6
C1 N1 Cr 123.69(18) . .
C1 N1 Cr 123.69(18) 6 .
C7 N2 C4 100(10) . .
C7 N2 Al 122.9(5) . .
C4 N2 Al 135(10) . .
C7 N2 Cr 72.1(3) . .
C4 N2 Cr 68(10) . .
Al N2 Cr 132.9(4) . .
C12 N3 C15 106.5(5) . .
C12 N3 Al 124.8(4) . .
C15 N3 Al 128.6(3) . .
N3 Al N2 101.3(2) . .
N3 Al C10 111.1(2) . .
N2 Al C10 111.5(3) . .
N3 Al C11 115.1(2) . .
N2 Al C11 106.9(3) . .
C10 Al C11 110.6(3) . .
C5 C4 N2 112(10) . .
C5 C4 C8 135(10) . .
N2 C4 C8 113(10) . .
C5 C4 Cr 77(10) . .
N2 C4 Cr 74(10) . .
C8 C4 Cr 117(10) . .
C4 C5 C6 110(10) . .
C4 C5 Cr 73(10) . .
C6 C5 Cr 73.8(5) . .
C5 C6 C7 107.9(9) . .
C5 C6 Cr 72.2(5) . .
C7 C6 Cr 72.4(4) . .
N2 C7 C6 109.5(6) . .
N2 C7 C9 123.2(7) . .
C6 C7 C9 127.2(7) . .
N2 C7 Cr 73.9(4) . .
C6 C7 Cr 72.9(3) . .
C9 C7 Cr 122.0(3) . .
C13 C12 N3 110.0(6) . .
C13 C12 C16 126.5(6) . .
N3 C12 C16 123.5(6) . .
C12 C13 C14 106.5(5) . .
C15 C14 C13 107.8(5) . .
C14 C15 N3 109.2(5) . .
C14 C15 C17 128.3(5) . .
N3 C15 C17 122.5(5) . .
C52 C51 C56 120.0 . .
C52 C51 C57 117.6(8) . .
C56 C51 C57 122.3(8) . .
C53 C52 C51 120.0 . .
C54 C53 C52 120.0 . .
C53 C54 C55 120.0 . .
C54 C55 C56 120.0 . .
C55 C56 C51 120.0 . .
N1 C1 C2 109.4(3) . .
N1 C1 C3 121.4(2) . .
C2 C1 C3 129.1(3) . .
C1 C2 C2 106.7(2) . 6
C1 C2 Cr 103.87(18) . 5_656
C2 C2 Cr 72.55(10) 6 5_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr N1 2.028(3) .
Cr C4 2(3) .
Cr C5 2.341(9) .
Cr C7 2.354(5) .
Cr C2 2.359(3) 5_656
Cr C2 2.359(3) 2_656
Cr C6 2.362(6) .
Cr N2 2.376(7) .
N1 C1 1.372(4) .
N1 C1 1.372(4) 6
N2 C7 1.382(10) .
N2 C4 2(10) .
N2 Al 1.957(7) .
N3 C12 1.384(8) .
N3 C15 1.391(6) .
N3 Al 1.912(4) .
Al C10 1.971(7) .
Al C11 1.991(5) .
C4 C5 1(10) .
C4 C8 2(10) .
C5 C6 1.377(9) .
C6 C7 1.407(12) .
C7 C9 1.489(7) .
C12 C13 1.373(9) .
C12 C16 1.487(9) .
C13 C14 1.415(8) .
C14 C15 1.368(7) .
C15 C17 1.493(8) .
C57 C51 1.555(12) .
C51 C52 1.3900 .
C51 C56 1.3900 .
C52 C53 1.3900 .
C53 C54 1.3900 .
C54 C55 1.3900 .
C55 C56 1.3900 .
C1 C2 1.386(4) .
C1 C3 1.491(5) .
C2 C2 1.415(8) 6
C2 Cr 2.359(3) 5_656
