#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:38:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178609 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/20/4072066.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_4072066
loop_
_publ_author_name
'Albahily, Khalid'
'Al-Baldawi, Danya'
'Gambarotta, Sandro'
'Duchateau, Robbert'
'Koç, Ece'
'Burchell, Tara J.'
_publ_section_title
;
 Preparation and Characterization of a Switchable Single-Component
 Chromium Trimerization Catalyst
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5708
_journal_paper_doi               10.1021/om800563w
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H52 Cr N4 P2'
_chemical_formula_weight         606.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.947(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.201(9)
_cell_length_b                   21.91(2)
_cell_length_c                   9.597(9)
_cell_measurement_reflns_used    4642
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      2.32
_cell_volume                     1768(3)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0856
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10360
_diffrn_reflns_theta_full        24.64
_diffrn_reflns_theta_max         24.64
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.9371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0559
_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)+(0.0757P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                2022
_reflns_number_total             2937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800563w_si_003.cif
_cod_data_source_block           sada
_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      P2(1)/n
_cod_database_code               4072066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 1.0000 0.0000 0.0000 0.0279(3) Uani 1 2 d S . .
N1 N 0.9574(3) 0.04726(12) 0.1718(3) 0.0303(7) Uani 1 1 d . . .
N2 N 1.0315(4) -0.05999(13) 0.1788(3) 0.0338(7) Uani 1 1 d . A .
P1 P 0.99102(13) -0.01153(4) 0.28431(11) 0.0369(3) Uani 1 1 d . . .
C1 C 0.9215(4) 0.10675(14) 0.2116(4) 0.0298(8) Uani 1 1 d . . .
C2 C 0.7613(4) 0.12473(16) 0.1716(4) 0.0343(9) Uani 1 1 d . . .
C3 C 0.7309(5) 0.18417(17) 0.2044(5) 0.0432(10) Uani 1 1 d . . .
H3A H 0.6252 0.1966 0.1781 0.052 Uiso 1 1 calc R . .
C4 C 0.8530(5) 0.22519(17) 0.2748(5) 0.0464(11) Uani 1 1 d . . .
H4A H 0.8300 0.2652 0.2951 0.056 Uiso 1 1 calc R . .
C5 C 1.0090(5) 0.20727(16) 0.3153(4) 0.0417(10) Uani 1 1 d . . .
H5A H 1.0912 0.2355 0.3637 0.050 Uiso 1 1 calc R . .
C6 C 1.0478(4) 0.14838(16) 0.2861(4) 0.0343(9) Uani 1 1 d . . .
C7 C 0.6251(4) 0.07867(17) 0.1007(5) 0.0429(10) Uani 1 1 d . . .
H7A H 0.6610 0.0470 0.0482 0.051 Uiso 1 1 calc R . .
C8 C 0.5890(6) 0.0471(2) 0.2257(6) 0.0625(13) Uani 1 1 d . . .
H8A H 0.5047 0.0174 0.1798 0.094 Uiso 1 1 calc R . .
H8B H 0.5558 0.0773 0.2807 0.094 Uiso 1 1 calc R . .
H8C H 0.6839 0.0265 0.2959 0.094 Uiso 1 1 calc R . .
C9 C 0.4721(5) 0.1076(2) -0.0181(5) 0.0651(14) Uani 1 1 d . . .
H9A H 0.3962 0.0757 -0.0697 0.098 Uiso 1 1 calc R . .
H9B H 0.4975 0.1303 -0.0921 0.098 Uiso 1 1 calc R . .
H9C H 0.4265 0.1350 0.0328 0.098 Uiso 1 1 calc R . .
C10 C 1.2219(5) 0.12900(18) 0.3357(5) 0.0449(10) Uani 1 1 d . . .
H10A H 1.2252 0.0974 0.2633 0.054 Uiso 1 1 calc R . .
C11 C 1.3328(5) 0.18107(19) 0.3337(6) 0.0622(13) Uani 1 1 d . . .
H11A H 1.4363 0.1645 0.3502 0.093 Uiso 1 1 calc R . .
H11B H 1.3440 0.2100 0.4139 0.093 Uiso 1 1 calc R . .
H11C H 1.2881 0.2016 0.2357 0.093 Uiso 1 1 calc R . .
C12 C 1.2883(6) 0.1002(2) 0.4962(6) 0.0682(14) Uani 1 1 d . . .
H12A H 1.3945 0.0846 0.5202 0.102 Uiso 1 1 calc R . .
H12B H 1.2196 0.0670 0.4986 0.102 Uiso 1 1 calc R . .
H12C H 1.2926 0.1308 0.5707 0.102 Uiso 1 1 calc R . .
C13 C 1.0795(5) -0.12465(16) 0.2238(4) 0.0392(9) Uani 1 1 d . . .
C14 C 0.9581(5) -0.16590(17) 0.1020(5) 0.0558(12) Uani 1 1 d . A .
H14A H 0.9550 -0.1556 0.0025 0.084 Uiso 1 1 calc R . .
H14B H 0.8536 -0.1598 0.1018 0.084 Uiso 1 1 calc R . .
H14C H 0.9892 -0.2083 0.1249 0.084 Uiso 1 1 calc R . .
C15 C 1.2435(5) -0.13368(19) 0.2221(6) 0.0607(13) Uani 1 1 d . A .
H15A H 1.3198 -0.1072 0.2975 0.091 Uiso 1 1 calc R . .
H15B H 1.2387 -0.1237 0.1219 0.091 Uiso 1 1 calc R . .
H15C H 1.2761 -0.1759 0.2460 0.091 Uiso 1 1 calc R . .
C16 C 1.0508(14) -0.1435(5) 0.3667(13) 0.045(3) Uani 0.50 1 d PU A 1
H16A H 1.1158 -0.1184 0.4528 0.067 Uiso 0.50 1 calc PR A 1
H16B H 1.0790 -0.1861 0.3900 0.067 Uiso 0.50 1 calc PR A 1
H16C H 0.9395 -0.1378 0.3465 0.067 Uiso 0.50 1 calc PR A 1
C16A C 1.1270(14) -0.1354(7) 0.4001(15) 0.056(4) Uani 0.50 1 d PU A 2
H16D H 1.2135 -0.1083 0.4587 0.085 Uiso 0.50 1 calc PR A 2
H16E H 1.1606 -0.1774 0.4257 0.085 Uiso 0.50 1 calc PR A 2
H16F H 1.0360 -0.1272 0.4239 0.085 Uiso 0.50 1 calc PR A 2
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'
P P 0.1023 0.0942 '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
N2 Cr1 N2 179.998(1) . 3_755
N2 Cr1 N1 108.98(13) . 3_755
N2 Cr1 N1 71.02(13) 3_755 3_755
N2 Cr1 N1 71.02(13) . .
N2 Cr1 N1 108.98(13) 3_755 .
N1 Cr1 N1 180.0 3_755 .
N2 Cr1 P1 35.25(8) . .
N2 Cr1 P1 144.74(8) 3_755 .
N1 Cr1 P1 144.23(9) 3_755 .
N1 Cr1 P1 35.77(9) . .
N2 Cr1 P1 144.75(8) . 3_755
N2 Cr1 P1 35.26(8) 3_755 3_755
N1 Cr1 P1 35.77(9) 3_755 3_755
N1 Cr1 P1 144.23(9) . 3_755
P1 Cr1 P1 180.0 . 3_755
C1 N1 P1 123.0(2) . .
C1 N1 Cr1 142.0(2) . .
P1 N1 Cr1 94.84(14) . .
C13 N2 P1 124.0(2) . .
C13 N2 Cr1 139.5(2) . .
P1 N2 Cr1 96.40(16) . .
N2 P1 N1 97.73(16) . .
N2 P1 Cr1 48.35(11) . .
N1 P1 Cr1 49.39(10) . .
C2 C1 C6 120.3(3) . .
C2 C1 N1 120.4(3) . .
C6 C1 N1 119.2(3) . .
C3 C2 C1 118.6(3) . .
C3 C2 C7 120.7(3) . .
C1 C2 C7 120.5(3) . .
C4 C3 C2 121.3(4) . .
C3 C4 C5 119.8(3) . .
C4 C5 C6 121.7(4) . .
C5 C6 C1 118.1(3) . .
C5 C6 C10 120.9(3) . .
C1 C6 C10 121.1(3) . .
C8 C7 C2 110.2(3) . .
C8 C7 C9 110.0(4) . .
C2 C7 C9 113.1(3) . .
C6 C10 C11 113.9(3) . .
C6 C10 C12 111.3(3) . .
C11 C10 C12 108.7(4) . .
N2 C13 C15 107.3(3) . .
N2 C13 C14 107.4(3) . .
C15 C13 C14 109.3(3) . .
N2 C13 C16 111.7(5) . .
C15 C13 C16 119.8(5) . .
C14 C13 C16 100.5(5) . .
N2 C13 C16A 111.8(6) . .
C15 C13 C16A 98.4(5) . .
C14 C13 C16A 121.6(6) . .
C16 C13 C16A 24.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N2 2.086(3) .
Cr1 N2 2.086(3) 3_755
Cr1 N1 2.114(3) 3_755
Cr1 N1 2.114(3) .
Cr1 P1 2.775(3) .
Cr1 P1 2.775(3) 3_755
N1 C1 1.434(4) .
N1 P1 1.628(3) .
N2 C13 1.495(5) .
N2 P1 1.612(3) .
C1 C2 1.420(5) .
C1 C6 1.421(5) .
C2 C3 1.394(5) .
C2 C7 1.536(5) .
C3 C4 1.382(6) .
C4 C5 1.384(5) .
C5 C6 1.397(5) .
C6 C10 1.534(5) .
C7 C8 1.534(6) .
C7 C9 1.542(6) .
C10 C11 1.536(5) .
C10 C12 1.543(6) .
C13 C15 1.528(5) .
C13 C14 1.540(6) .
C13 C16 1.555(13) .
C13 C16A 1.584(14) .
