#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:14:00 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178554 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/62/4066252.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_4066252
loop_
_publ_author_name
'Peitz, Stephan'
'Peulecke, Normen'
'Aluri, Bhaskar R.'
'Müller, Bernd H.'
'Spannenberg, Anke'
'Rosenthal, Uwe'
'Al-Hazmi, Mohammed H.'
'Mosa, Fuad M.'
'Wöhl, Anina'
'Müller, Wolfgang'
_publ_section_title
;
 Metalation and Transmetalation Studies on Ph2PN(iPr)P(Ph)N(iPr)H for
 Selective Ethene Trimerization to 1-Hexene⊥
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5263
_journal_paper_doi               10.1021/om100371f
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C14 H29 Cl2 Cr O3'
_chemical_formula_weight         368.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.220(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9517(3)
_cell_length_b                   13.2013(3)
_cell_length_c                   14.9130(5)
_cell_measurement_reflns_used    10433
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      1.49
_cell_volume                     1761.93(9)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       ω
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0129
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26361
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.7808
_exptl_absorpt_correction_T_min  0.6972
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED32 (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3742
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0462P)²+0.3633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3173
_reflns_number_total             3742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100371f_si_001.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4066252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 1.0401(2) 0.21576(17) 0.15504(15) 0.0501(5) Uani 1 1 d . . .
H1A H 1.0270 0.1416 0.1490 0.060 Uiso 1 1 calc R . .
H1B H 1.0986 0.2299 0.2107 0.060 Uiso 1 1 calc R . .
C2 C 1.1174(2) 0.25849(17) 0.07458(15) 0.0484(5) Uani 1 1 d . . .
H2A H 1.0906 0.2202 0.0195 0.058 Uiso 1 1 calc R . .
H2B H 1.2273 0.2577 0.0834 0.058 Uiso 1 1 calc R . .
C3 C 1.0584(2) 0.36536(15) 0.07001(13) 0.0398(4) Uani 1 1 d . . .
H3A H 1.1114 0.4099 0.1136 0.048 Uiso 1 1 calc R . .
H3B H 1.0673 0.3940 0.0090 0.048 Uiso 1 1 calc R . .
C4 C 0.8974(2) 0.35136(15) 0.09423(13) 0.0412(4) Uani 1 1 d . . .
H4A H 0.8582 0.4132 0.1229 0.049 Uiso 1 1 calc R . .
H4B H 0.8354 0.3361 0.0401 0.049 Uiso 1 1 calc R . .
C5 C 0.7048(2) -0.01706(14) 0.19366(14) 0.0459(5) Uani 1 1 d . . .
H5A H 0.6225 -0.0255 0.2363 0.055 Uiso 1 1 calc R . .
H5B H 0.8005 -0.0326 0.2252 0.055 Uiso 1 1 calc R . .
C6 C 0.6822(3) -0.08597(17) 0.11391(16) 0.0561(5) Uani 1 1 d . . .
H6A H 0.5755 -0.1039 0.1054 0.067 Uiso 1 1 calc R . .
H6B H 0.7414 -0.1489 0.1210 0.067 Uiso 1 1 calc R . .
C7 C 0.7368(3) -0.02341(18) 0.03629(15) 0.0565(6) Uani 1 1 d . . .
H7A H 0.8461 -0.0307 0.0296 0.068 Uiso 1 1 calc R . .
H7B H 0.6859 -0.0433 -0.0206 0.068 Uiso 1 1 calc R . .
C8 C 0.6967(3) 0.08231(17) 0.06215(13) 0.0525(5) Uani 1 1 d . . .
H8A H 0.7673 0.1315 0.0362 0.063 Uiso 1 1 calc R . .
H8B H 0.5942 0.0991 0.0408 0.063 Uiso 1 1 calc R . .
C9 C 0.40098(18) 0.14997(15) 0.27185(11) 0.0371(4) Uani 1 1 d D . .
H9A H 0.4076 0.1137 0.2140 0.045 Uiso 0.718(8) 1 calc PR A 1
H9B H 0.3468 0.2145 0.2618 0.045 Uiso 0.718(8) 1 calc PR A 1
H9C H 0.4048 0.0955 0.2263 0.045 Uiso 0.282(8) 1 calc PR A 2
H9D H 0.3610 0.2121 0.2429 0.045 Uiso 0.282(8) 1 calc PR A 2
C12 C 0.5535(2) 0.13694(19) 0.40362(12) 0.0509(6) Uani 1 1 d D . .
H12A H 0.5992 0.1901 0.4421 0.061 Uiso 0.718(8) 1 calc PR A 1
H12B H 0.6119 0.0737 0.4111 0.061 Uiso 0.718(8) 1 calc PR A 1
H12C H 0.5619 0.1966 0.4436 0.061 Uiso 0.282(8) 1 calc PR A 2
H12D H 0.6405 0.0922 0.4154 0.061 Uiso 0.282(8) 1 calc PR A 2
C13 C 0.7393(2) 0.35345(15) 0.31914(12) 0.0397(4) Uani 1 1 d . A .
H13A H 0.6707 0.4052 0.2934 0.048 Uiso 1 1 calc R . .
H13B H 0.7021 0.3357 0.3792 0.048 Uiso 1 1 calc R . .
C14 C 0.8913(3) 0.40122(19) 0.33139(16) 0.0594(6) Uani 1 1 d . . .
H14A H 0.8837 0.4608 0.3703 0.089 Uiso 1 1 calc R . .
H14B H 0.9287 0.4219 0.2729 0.089 Uiso 1 1 calc R . .
H14C H 0.9603 0.3521 0.3590 0.089 Uiso 1 1 calc R . .
Cl1 Cl 0.89163(4) 0.14089(4) 0.33503(3) 0.03983(12) Uani 1 1 d . A .
Cl2 Cl 0.55616(4) 0.30230(4) 0.13897(3) 0.03835(12) Uani 1 1 d . A .
Cr1 Cr 0.72501(3) 0.225749(19) 0.239469(16) 0.02502(8) Uani 1 1 d . . .
O1 O 0.89654(12) 0.26612(9) 0.15671(8) 0.0307(2) Uani 1 1 d . A .
O2 O 0.70643(15) 0.08456(9) 0.15889(8) 0.0390(3) Uani 1 1 d . A .
O3 O 0.54892(12) 0.16871(10) 0.30999(7) 0.0318(3) Uani 1 1 d . A .
C10A C 0.3228(4) 0.0859(3) 0.33966(13) 0.0386(8) Uiso 0.718(8) 1 d PD A 1
H10A H 0.3408 0.0129 0.3292 0.046 Uiso 0.718(8) 1 calc PR A 1
H10B H 0.2138 0.0988 0.3383 0.046 Uiso 0.718(8) 1 calc PR A 1
C11A C 0.3934(2) 0.1202(3) 0.42698(16) 0.0390(8) Uiso 0.718(8) 1 d PD A 1
H11A H 0.3470 0.1836 0.4483 0.047 Uiso 0.718(8) 1 calc PR A 1
H11B H 0.3844 0.0676 0.4738 0.047 Uiso 0.718(8) 1 calc PR A 1
C10B C 0.3039(5) 0.1187(7) 0.3481(3) 0.0342(19) Uiso 0.282(8) 1 d PD A 2
H10C H 0.2454 0.1770 0.3700 0.041 Uiso 0.282(8) 1 calc PR A 2
H10D H 0.2339 0.0644 0.3290 0.041 Uiso 0.282(8) 1 calc PR A 2
C11B C 0.4104(4) 0.0810(6) 0.4198(4) 0.0300(18) Uiso 0.282(8) 1 d PD A 2
H11C H 0.4253 0.0070 0.4145 0.036 Uiso 0.282(8) 1 calc PR A 2
H11D H 0.3725 0.0964 0.4802 0.036 Uiso 0.282(8) 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'
O O 0.0106 0.0060 '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
O1 C1 C2 105.35(15)
C1 C2 C3 102.70(15)
C4 C3 C2 102.16(15)
O1 C4 C3 105.43(14)
O2 C5 C6 106.30(16)
C5 C6 C7 103.54(17)
C8 C7 C6 103.25(18)
O2 C8 C7 105.52(18)
O3 C9 C10A 105.45(15)
O3 C9 C10B 106.7(2)
O3 C12 C11A 104.92(15)
O3 C12 C11B 106.7(2)
C14 C13 Cr1 117.13(14)
O3 Cr1 O1 171.97(5)
O3 Cr1 C13 92.49(6)
O1 Cr1 C13 95.49(6)
O3 Cr1 O2 85.42(5)
O1 Cr1 O2 86.63(5)
C13 Cr1 O2 177.52(6)
O3 Cr1 Cl1 89.93(3)
O1 Cr1 Cl1 90.87(3)
C13 Cr1 Cl1 90.55(6)
O2 Cr1 Cl1 88.11(4)
O3 Cr1 Cl2 89.65(3)
O1 Cr1 Cl2 89.09(3)
C13 Cr1 Cl2 92.71(6)
O2 Cr1 Cl2 88.62(4)
Cl1 Cr1 Cl2 176.73(2)
C1 O1 C4 109.01(13)
C1 O1 Cr1 124.38(10)
C4 O1 Cr1 126.55(9)
C5 O2 C8 109.88(15)
C5 O2 Cr1 126.05(11)
C8 O2 Cr1 124.05(12)
C9 O3 C12 109.47(12)
C9 O3 Cr1 124.40(9)
C12 O3 Cr1 126.09(9)
C9 C10A C11A 102.71(18)
C12 C11A C10A 103.27(19)
C11B C10B C9 105.1(3)
C10B C11B C12 104.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.447(2)
C1 C2 1.507(3)
C2 C3 1.507(3)
C3 C4 1.504(2)
C4 O1 1.461(2)
C5 O2 1.438(2)
C5 C6 1.508(3)
C6 C7 1.512(3)
C7 C8 1.494(3)
C8 O2 1.444(2)
C9 O3 1.4515(19)
C9 C10A 1.5025(19)
C9 C10B 1.504(2)
C12 O3 1.4576(19)
C12 C11A 1.4984(19)
C12 C11B 1.503(2)
C13 C14 1.507(3)
C13 Cr1 2.0649(18)
Cl1 Cr1 2.3281(5)
Cl2 Cr1 2.3358(5)
Cr1 O3 2.0563(11)
Cr1 O1 2.0604(11)
Cr1 O2 2.2220(13)
C10A C11A 1.5050(19)
C10B C11B 1.502(2)
