#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:19:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178503 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/50/4065094.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_4065094
loop_
_publ_author_name
'Albahily, Khalid'
'Fomitcheva, Valeria'
'Shaikh, Yacoob'
'Sebastiao, Elena'
'Gorelsky, Serge I.'
'Gambarotta, Sandro'
'Korobkov, Ilia'
'Duchateau, Robbert'
_publ_section_title
;
 New Self-Activating Organochromium Catalyst Precursor for Selective
 Ethylene Trimerization.
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4201
_journal_paper_doi               10.1021/om200560e
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C22 H52 Cr Li N4 O P2'
_chemical_formula_weight         509.56
_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                 92.6750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1079(11)
_cell_length_b                   17.0588(17)
_cell_length_c                   16.0537(16)
_cell_measurement_reflns_used    6755
_cell_measurement_temperature    201(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.19
_cell_volume                     3038.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      201(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10764
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9517
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Dark_blue
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0571P)²+4.7554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                2453
_reflns_number_total             3087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200560e_si_002.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4065094
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 0.5000 0.26474(3) 0.2500 0.02917(17) Uani 1 2 d S . .
P2 P 0.67572(6) 0.24130(4) 0.13917(4) 0.0405(2) Uani 1 1 d . . .
N1 N 0.63720(18) 0.19086(12) 0.22782(14) 0.0358(5) Uani 1 1 d . . .
N2 N 0.55642(19) 0.30397(12) 0.14801(13) 0.0368(5) Uani 1 1 d . . .
C14 C 0.6278(3) 0.1715(2) 0.0565(2) 0.0601(8) Uani 1 1 d . . .
H14A H 0.5441 0.1558 0.0638 0.090 Uiso 1 1 calc R . .
H14B H 0.6799 0.1251 0.0597 0.090 Uiso 1 1 calc R . .
H14C H 0.6340 0.1965 0.0019 0.090 Uiso 1 1 calc R . .
Li2 Li 0.5000 0.1101(4) 0.2500 0.0495(16) Uani 1 2 d S . .
O1 O 0.5000 -0.00274(17) 0.2500 0.0759(11) Uani 1 2 d SD . .
C10 C 0.5876(7) -0.0334(5) 0.1891(5) 0.064(2) Uani 0.50 1 d PD A -1
H10A H 0.6378 0.0102 0.1693 0.077 Uiso 0.50 1 calc PR A -1
H10B H 0.6416 -0.0726 0.2168 0.077 Uiso 0.50 1 calc PR A -1
C11 C 0.5197(11) -0.0701(7) 0.1170(6) 0.079(3) Uani 0.50 1 d PD A -1
H11A H 0.5765 -0.0887 0.0764 0.118 Uiso 0.50 1 calc PR A -1
H11B H 0.4652 -0.0314 0.0904 0.118 Uiso 0.50 1 calc PR A -1
H11C H 0.4727 -0.1145 0.1366 0.118 Uiso 0.50 1 calc PR A -1
C12 C 0.4812(11) -0.0685(4) 0.2979(6) 0.092(3) Uani 0.50 1 d PD A -1
H12A H 0.5568 -0.0986 0.3072 0.111 Uiso 0.50 1 calc PR A -1
H12B H 0.4195 -0.1030 0.2706 0.111 Uiso 0.50 1 calc PR A -1
C13 C 0.4393(14) -0.0379(7) 0.3773(9) 0.115(6) Uani 0.50 1 d PD A -1
H13A H 0.4231 -0.0817 0.4146 0.172 Uiso 0.50 1 calc PR A -1
H13B H 0.3653 -0.0075 0.3667 0.172 Uiso 0.50 1 calc PR A -1
H13C H 0.5016 -0.0041 0.4034 0.172 Uiso 0.50 1 calc PR A -1
C1 C 0.7413(2) 0.17407(16) 0.2874(2) 0.0469(7) Uani 1 1 d . . .
C2 C 0.8277(3) 0.1174(2) 0.2482(3) 0.0740(11) Uani 1 1 d . . .
H2A H 0.7862 0.0678 0.2358 0.111 Uiso 1 1 calc R . .
H2B H 0.8969 0.1079 0.2870 0.111 Uiso 1 1 calc R . .
H2C H 0.8558 0.1400 0.1964 0.111 Uiso 1 1 calc R . .
C3 C 0.6931(3) 0.1358(2) 0.3652(2) 0.0595(8) Uani 1 1 d . . .
H3A H 0.6544 0.0859 0.3499 0.089 Uiso 1 1 calc R . .
H3B H 0.6341 0.1706 0.3896 0.089 Uiso 1 1 calc R . .
H3C H 0.7599 0.1263 0.4060 0.089 Uiso 1 1 calc R . .
C4 C 0.8099(3) 0.2480(2) 0.3141(3) 0.0750(12) Uani 1 1 d . . .
H4A H 0.8374 0.2751 0.2646 0.113 Uiso 1 1 calc R . .
H4B H 0.8797 0.2337 0.3505 0.113 Uiso 1 1 calc R . .
H4C H 0.7567 0.2827 0.3442 0.113 Uiso 1 1 calc R . .
C5 C 0.5380(3) 0.37387(16) 0.09477(17) 0.0434(6) Uani 1 1 d . . .
C6 C 0.6469(3) 0.42717(18) 0.1029(2) 0.0612(8) Uani 1 1 d . . .
H6A H 0.6576 0.4454 0.1606 0.092 Uiso 1 1 calc R . .
H6B H 0.6348 0.4723 0.0657 0.092 Uiso 1 1 calc R . .
H6C H 0.7188 0.3982 0.0876 0.092 Uiso 1 1 calc R . .
C7 C 0.5172(4) 0.3505(2) 0.0034(2) 0.0675(10) Uani 1 1 d . . .
H7A H 0.5898 0.3252 -0.0162 0.101 Uiso 1 1 calc R . .
H7B H 0.4990 0.3973 -0.0302 0.101 Uiso 1 1 calc R . .
H7C H 0.4493 0.3139 -0.0020 0.101 Uiso 1 1 calc R . .
C8 C 0.4276(4) 0.4173(2) 0.1233(3) 0.0832(13) Uani 1 1 d . . .
H8A H 0.3556 0.3851 0.1120 0.125 Uiso 1 1 calc R . .
H8B H 0.4190 0.4670 0.0931 0.125 Uiso 1 1 calc R . .
H8C H 0.4371 0.4277 0.1833 0.125 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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
N2 Cr1 N2 138.79(13) . 2_655
N2 Cr1 N1 77.67(8) . .
N2 Cr1 N1 130.71(9) 2_655 .
N2 Cr1 N1 130.72(9) . 2_655
N2 Cr1 N1 77.67(8) 2_655 2_655
N1 Cr1 N1 102.89(12) . 2_655
N2 Cr1 Li2 110.61(6) . .
N2 Cr1 Li2 110.60(6) 2_655 .
N1 Cr1 Li2 51.45(6) . .
N1 Cr1 Li2 51.45(6) 2_655 .
N2 Cr1 P2 38.42(6) . .
N2 Cr1 P2 152.44(7) 2_655 .
N1 Cr1 P2 39.34(6) . .
N1 Cr1 P2 126.23(6) 2_655 .
Li2 Cr1 P2 81.583(18) . .
N2 Cr1 P2 152.44(7) . 2_655
N2 Cr1 P2 38.42(6) 2_655 2_655
N1 Cr1 P2 126.23(6) . 2_655
N1 Cr1 P2 39.34(6) 2_655 2_655
Li2 Cr1 P2 81.583(18) . 2_655
P2 Cr1 P2 163.17(4) . 2_655
N2 P2 N1 91.16(10) . .
N2 P2 C14 105.33(14) . .
N1 P2 C14 101.35(13) . .
N2 P2 Cr1 43.60(7) . .
N1 P2 Cr1 47.67(7) . .
C14 P2 Cr1 111.89(11) . .
C1 N1 P2 114.07(16) . .
C1 N1 Cr1 125.02(18) . .
P2 N1 Cr1 92.99(9) . .
C1 N1 Li2 108.20(16) . .
P2 N1 Li2 132.42(13) . .
Cr1 N1 Li2 79.60(15) . .
C5 N2 P2 122.90(17) . .
C5 N2 Cr1 137.77(17) . .
P2 N2 Cr1 97.98(10) . .
O1 Li2 N1 131.05(14) . 2_655
O1 Li2 N1 131.05(14) . .
N1 Li2 N1 97.9(3) 2_655 .
O1 Li2 Cr1 180.0 . .
N1 Li2 Cr1 48.95(14) 2_655 .
N1 Li2 Cr1 48.95(14) . .
C12 O1 C12 71.5(7) 2_655 .
C12 O1 C10 40.3(4) 2_655 .
C12 O1 C10 101.5(7) . .
C12 O1 C10 101.5(7) 2_655 2_655
C12 O1 C10 40.3(4) . 2_655
C10 O1 C10 139.4(8) . 2_655
C12 O1 Li2 144.3(4) 2_655 .
C12 O1 Li2 144.3(4) . .
C10 O1 Li2 110.3(4) . .
C10 O1 Li2 110.3(4) 2_655 .
C11 C10 O1 109.4(7) . .
O1 C12 C13 104.8(8) . .
N1 C1 C2 110.0(3) . .
N1 C1 C4 112.5(2) . .
C2 C1 C4 109.0(3) . .
N1 C1 C3 108.4(2) . .
C2 C1 C3 108.6(3) . .
C4 C1 C3 108.3(3) . .
N2 C5 C6 110.3(2) . .
N2 C5 C8 108.1(2) . .
C6 C5 C8 109.5(3) . .
N2 C5 C7 110.8(2) . .
C6 C5 C7 108.9(3) . .
C8 C5 C7 109.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N2 1.902(2) .
Cr1 N2 1.902(2) 2_655
Cr1 N1 2.022(2) .
Cr1 N1 2.022(2) 2_655
Cr1 Li2 2.637(6) .
Cr1 P2 2.7311(7) .
Cr1 P2 2.7312(7) 2_655
P2 N2 1.714(2) .
P2 N1 1.734(2) .
P2 C14 1.843(3) .
N1 C1 1.494(3) .
N1 Li2 2.097(5) .
N2 C5 1.476(3) .
Li2 O1 1.926(7) .
Li2 N1 2.097(5) 2_655
O1 C12 1.382(7) 2_655
O1 C12 1.382(7) .
O1 C10 1.505(7) .
O1 C10 1.505(7) 2_655
C10 C11 1.490(8) .
C12 C13 1.472(9) .
C1 C2 1.520(4) .
C1 C4 1.524(4) .
C1 C3 1.528(4) .
C5 C6 1.514(4) .
C5 C8 1.521(4) .
C5 C7 1.527(4) .
