#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:52:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178671 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/82/4078275.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_4078275
loop_
_publ_author_name
'Müller, Bernd H.'
'Peulecke, Normen'
'Spannenberg, Anke'
'Rosenthal, Uwe'
'Al-Hazmi, Mohammed H.'
'Schmidt, Roland'
'Wöhl, Anina'
'Müller, Wolfgang'
_publ_section_title
;
 Synthesis and Reactions of the Homoleptic Chromium(II) Bis-amide
 [Ph2PN(iPr)P(Ph)N(iPr)−]2Cr with Relevance to a Selective
 Catalytic Ethene Trimerization System to 1-Hexene
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3695
_journal_paper_doi               10.1021/om300186a
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C59 H76 Al2 Cl6 Cr2 N4 P4'
_chemical_formula_weight         1335.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.7700(10)
_cell_angle_beta                 98.9660(10)
_cell_angle_gamma                112.3520(10)
_cell_formula_units_Z            1
_cell_length_a                   10.7903(2)
_cell_length_b                   11.4254(2)
_cell_length_c                   14.7974(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.05
_cell_measurement_theta_min      2.47
_cell_volume                     1661.31(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 V2011.4-1 (Bruker AXS, 2011)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38102
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.8336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0385
_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)+(0.0527P)²+1.9247P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                6581
_reflns_number_total             7602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300186a_si_002.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        1661.30(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.15895(6) 0.50799(7) 0.26275(5) 0.02629(15) Uani 1 1 d . . .
C1 C 0.2581(2) 0.5222(3) 0.08685(15) 0.0330(5) Uani 1 1 d . . .
H1 H 0.3295 0.5036 0.0609 0.040 Uiso 1 1 calc R . .
C2 C 0.1205(3) 0.4144(3) 0.05201(17) 0.0410(6) Uani 1 1 d . . .
H2A H 0.1231 0.3340 0.0724 0.062 Uiso 1 1 calc R . .
H2B H 0.1013 0.4092 -0.0152 0.062 Uiso 1 1 calc R . .
H2C H 0.0490 0.4311 0.0766 0.062 Uiso 1 1 calc R . .
C3 C 0.2569(3) 0.6468(3) 0.05308(19) 0.0449(7) Uani 1 1 d . . .
H3A H 0.1857 0.6656 0.0764 0.067 Uiso 1 1 calc R . .
H3B H 0.2386 0.6399 -0.0142 0.067 Uiso 1 1 calc R . .
H3C H 0.3455 0.7152 0.0753 0.067 Uiso 1 1 calc R . .
C4 C 0.4925(2) 0.4258(2) 0.19381(14) 0.0255(4) Uani 1 1 d . . .
C5 C 0.3933(3) 0.3118(2) 0.15122(16) 0.0322(5) Uani 1 1 d . . .
H5 H 0.3007 0.3021 0.1379 0.039 Uiso 1 1 calc R . .
C6 C 0.4295(3) 0.2126(2) 0.12825(19) 0.0411(6) Uani 1 1 d . . .
H6 H 0.3613 0.1354 0.0990 0.049 Uiso 1 1 calc R . .
C7 C 0.5629(3) 0.2243(3) 0.1472(2) 0.0435(6) Uani 1 1 d . . .
H7 H 0.5869 0.1563 0.1302 0.052 Uiso 1 1 calc R . .
C8 C 0.6624(3) 0.3366(3) 0.1915(2) 0.0414(6) Uani 1 1 d . . .
H8 H 0.7545 0.3451 0.2057 0.050 Uiso 1 1 calc R . .
C9 C 0.6264(2) 0.4358(2) 0.21486(17) 0.0318(5) Uani 1 1 d . . .
H9 H 0.6944 0.5119 0.2457 0.038 Uiso 1 1 calc R . .
C10 C 0.6151(2) 0.7372(2) 0.14015(15) 0.0299(5) Uani 1 1 d . . .
H10 H 0.5418 0.6838 0.0892 0.036 Uiso 1 1 calc R . .
C11 C 0.7458(3) 0.7220(3) 0.12677(18) 0.0377(5) Uani 1 1 d . . .
H11A H 0.8174 0.7641 0.1797 0.057 Uiso 1 1 calc R . .
H11B H 0.7746 0.7607 0.0709 0.057 Uiso 1 1 calc R . .
H11C H 0.7294 0.6316 0.1211 0.057 Uiso 1 1 calc R . .
C12 C 0.6295(3) 0.8744(2) 0.13024(18) 0.0387(6) Uani 1 1 d . . .
H12A H 0.5429 0.8814 0.1347 0.058 Uiso 1 1 calc R . .
H12B H 0.6542 0.8999 0.0704 0.058 Uiso 1 1 calc R . .
H12C H 0.7006 0.9300 0.1792 0.058 Uiso 1 1 calc R . .
C13 C 0.8107(2) 0.8254(3) 0.35995(16) 0.0341(5) Uani 1 1 d . . .
C14 C 0.8684(3) 0.7419(3) 0.39402(19) 0.0429(6) Uani 1 1 d . . .
H14 H 0.8121 0.6597 0.4078 0.052 Uiso 1 1 calc R . .
C15 C 1.0095(3) 0.7786(4) 0.4081(2) 0.0609(10) Uani 1 1 d . . .
H15 H 1.0489 0.7208 0.4305 0.073 Uiso 1 1 calc R . .
C16 C 1.0909(3) 0.8973(5) 0.3899(2) 0.0734(13) Uani 1 1 d . . .
H16 H 1.1868 0.9214 0.3990 0.088 Uiso 1 1 calc R . .
C17 C 1.0354(3) 0.9818(4) 0.3586(3) 0.0715(12) Uani 1 1 d . . .
H17 H 1.0932 1.0650 0.3478 0.086 Uiso 1 1 calc R . .
C18 C 0.8945(3) 0.9468(3) 0.3423(2) 0.0507(7) Uani 1 1 d . . .
H18 H 0.8562 1.0052 0.3195 0.061 Uiso 1 1 calc R . .
C19 C 0.5757(2) 0.8969(2) 0.34227(16) 0.0295(5) Uani 1 1 d . . .
C20 C 0.6493(3) 1.0014(3) 0.4054(2) 0.0473(7) Uani 1 1 d . . .
H20 H 0.7323 1.0075 0.4422 0.057 Uiso 1 1 calc R . .
C21 C 0.6005(5) 1.0964(3) 0.4140(3) 0.0663(10) Uani 1 1 d . . .
H21 H 0.6510 1.1681 0.4565 0.080 Uiso 1 1 calc R . .
C22 C 0.4807(5) 1.0882(3) 0.3622(3) 0.0666(11) Uani 1 1 d . . .
H22 H 0.4490 1.1545 0.3680 0.080 Uiso 1 1 calc R . .
C23 C 0.4062(4) 0.9843(3) 0.3019(2) 0.0536(8) Uani 1 1 d . . .
H23 H 0.3224 0.9785 0.2665 0.064 Uiso 1 1 calc R . .
C24 C 0.4519(3) 0.8878(3) 0.29207(19) 0.0369(5) Uani 1 1 d . . .
H24 H 0.3986 0.8153 0.2510 0.044 Uiso 1 1 calc R . .
C25 C 0.0488(2) 0.3274(2) 0.28205(17) 0.0344(5) Uani 1 1 d . . .
H25A H -0.0199 0.2875 0.2264 0.041 Uiso 1 1 calc R . .
H25B H 0.1092 0.2800 0.2922 0.041 Uiso 1 1 calc R . .
C26 C -0.0223(5) 0.3195(4) 0.3641(3) 0.0838(14) Uani 1 1 d . . .
H26A H 0.0459 0.3520 0.4202 0.126 Uiso 1 1 calc R . .
H26B H -0.0807 0.2309 0.3693 0.126 Uiso 1 1 calc R . .
H26C H -0.0779 0.3705 0.3558 0.126 Uiso 1 1 calc R . .
Cl1 Cl 0.26666(6) 0.61020(6) 0.39941(4) 0.03254(13) Uani 1 1 d . . .
Cl2 Cl 0.40279(6) 0.35770(5) 0.43798(4) 0.03232(13) Uani 1 1 d . . .
Cl3 Cl 0.02854(7) 0.60571(7) 0.21437(5) 0.04444(17) Uani 1 1 d . . .
Cr1 Cr 0.49130(3) 0.57635(3) 0.40771(2) 0.02245(9) Uani 1 1 d . . .
N1 N 0.29253(18) 0.53020(18) 0.18975(12) 0.0254(4) Uani 1 1 d . . .
N2 N 0.57086(18) 0.68932(17) 0.22853(12) 0.0234(4) Uani 1 1 d . . .
P1 P 0.44463(5) 0.54704(5) 0.24132(3) 0.02121(12) Uani 1 1 d . . .
P2 P 0.62636(5) 0.76361(5) 0.33604(4) 0.02332(12) Uani 1 1 d . . .
C29 C 0.9615(7) 0.0316(6) 0.9690(5) 0.0873(13) Uani 0.50 1 d PGDU A -1
C30 C 0.9851(6) 0.0470(5) 1.0643(5) 0.0848(14) Uani 0.50 1 d PGU A -1
H30 H 0.9489 0.0973 1.0946 0.102 Uiso 0.50 1 calc PR A -1
C31 C 1.0618(6) -0.0111(6) 1.1154(4) 0.0854(14) Uani 0.50 1 d PGU A -1
H31 H 1.0779 -0.0006 1.1805 0.102 Uiso 0.50 1 calc PR A -1
C32 C 1.1149(6) -0.0847(6) 1.0711(5) 0.0895(15) Uani 0.50 1 d PGU A -1
H32 H 1.1673 -0.1244 1.1059 0.107 Uiso 0.50 1 calc PR A -1
C33 C 1.0912(6) -0.1001(5) 0.9758(5) 0.0892(15) Uani 0.50 1 d PGU A -1
H33 H 1.1275 -0.1504 0.9455 0.107 Uiso 0.50 1 calc PR A -1
C34 C 1.0146(7) -0.0420(6) 0.9247(4) 0.0870(14) Uani 0.50 1 d PGU A -1
H34 H 0.9984 -0.0525 0.8596 0.104 Uiso 0.50 1 calc PR A -1
C35 C 0.8975(12) 0.0966(10) 0.9082(9) 0.109(3) Uani 0.50 1 d PDU A -1
H35A H 0.8932 0.0685 0.8445 0.163 Uiso 0.50 1 calc PR A -1
H35B H 0.9503 0.1883 0.9185 0.163 Uiso 0.50 1 calc PR A -1
H35C H 0.8051 0.0775 0.9200 0.163 Uiso 0.50 1 calc PR A -1
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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_1
N1 Al1 C25 115.11(10) .
N1 Al1 Cl3 111.85(7) .
C25 Al1 Cl3 110.77(8) .
N1 Al1 Cl1 106.85(6) .
C25 Al1 Cl1 108.26(8) .
Cl3 Al1 Cl1 103.16(4) .
N1 C1 C3 111.4(2) .
N1 C1 C2 110.8(2) .
C3 C1 C2 110.0(2) .
C9 C4 C5 118.6(2) .
C9 C4 P1 119.56(17) .
C5 C4 P1 120.71(18) .
C6 C5 C4 120.2(2) .
C7 C6 C5 120.9(2) .
C6 C7 C8 119.5(2) .
C9 C8 C7 119.7(2) .
C8 C9 C4 121.1(2) .
N2 C10 C12 112.52(19) .
N2 C10 C11 112.47(19) .
C12 C10 C11 110.4(2) .
C14 C13 C18 119.5(3) .
C14 C13 P2 116.2(2) .
C18 C13 P2 124.3(2) .
C13 C14 C15 120.0(3) .
C16 C15 C14 120.2(4) .
C15 C16 C17 120.4(3) .
C16 C17 C18 120.5(4) .
C13 C18 C17 119.4(4) .
C24 C19 C20 119.1(2) .
C24 C19 P2 119.21(18) .
C20 C19 P2 121.2(2) .
C21 C20 C19 119.5(3) .
C22 C21 C20 120.8(3) .
C21 C22 C23 119.9(3) .
C22 C23 C24 120.6(3) .
C23 C24 C19 120.0(3) .
C26 C25 Al1 111.1(2) .
Al1 Cl1 Cr1 99.30(3) .
Cr1 Cl2 Cr1 87.36(2) 2_666
Cl2 Cr1 Cl2 92.64(2) 2_666
Cl2 Cr1 P1 163.97(3) 2_666
Cl2 Cr1 P1 97.91(2) .
Cl2 Cr1 P2 98.72(2) 2_666
Cl2 Cr1 P2 156.38(3) .
P1 Cr1 P2 67.25(2) .
Cl2 Cr1 Cl1 102.89(2) 2_666
Cl2 Cr1 Cl1 96.75(2) .
P1 Cr1 Cl1 87.88(2) .
P2 Cr1 Cl1 100.77(2) .
C1 N1 P1 121.00(15) .
C1 N1 Al1 121.06(14) .
P1 N1 Al1 117.77(10) .
C10 N2 P2 128.89(15) .
C10 N2 P1 126.50(14) .
P2 N2 P1 104.55(10) .
N1 P1 N2 114.42(9) .
N1 P1 C4 109.73(10) .
N2 P1 C4 105.64(10) .
N1 P1 Cr1 117.35(7) .
N2 P1 Cr1 93.88(6) .
C4 P1 Cr1 114.47(7) .
N2 P2 C19 109.67(10) .
N2 P2 C13 109.04(10) .
C19 P2 C13 107.59(12) .
N2 P2 Cr1 93.47(7) .
C19 P2 Cr1 115.01(8) .
C13 P2 Cr1 120.79(9) .
C30 C29 C34 120.0 .
C30 C29 C35 125.8(8) .
C34 C29 C35 113.9(8) .
C29 C30 C31 120.0 .
C32 C31 C30 120.0 .
C31 C32 C33 120.0 .
C32 C33 C34 120.0 .
C33 C34 C29 120.0 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al1 N1 1.8771(19) .
Al1 C25 2.001(2) .
Al1 Cl3 2.1545(9) .
Al1 Cl1 2.2305(8) .
C1 N1 1.503(3) .
C1 C3 1.518(4) .
C1 C2 1.530(3) .
C4 C9 1.390(3) .
C4 C5 1.395(3) .
C4 P1 1.820(2) .
C5 C6 1.386(4) .
C6 C7 1.377(4) .
C7 C8 1.392(4) .
C8 C9 1.386(3) .
C10 N2 1.501(3) .
C10 C12 1.527(3) .
C10 C11 1.527(3) .
C13 C14 1.385(4) .
C13 C18 1.392(4) .
C13 P2 1.812(2) .
C14 C15 1.397(4) .
C15 C16 1.364(6) .
C16 C17 1.368(6) .
C17 C18 1.397(4) .
C19 C24 1.389(4) .
C19 C20 1.395(3) .
C19 P2 1.809(2) .
C20 C21 1.387(5) .
C21 C22 1.366(6) .
C22 C23 1.368(6) .
C23 C24 1.383(4) .
C25 C26 1.521(5) .
Cl1 Cr1 2.5810(6) .
Cl2 Cr1 2.3608(6) 2_666
Cl2 Cr1 2.3879(6) .
Cr1 Cl2 2.3609(6) 2_666
Cr1 P1 2.4271(6) .
Cr1 P2 2.4489(7) .
N1 P1 1.6366(18) .
N2 P2 1.7000(18) .
N2 P1 1.7140(18) .
C29 C30 1.3900 .
C29 C34 1.3900 .
C29 C35 1.433(8) .
C30 C31 1.3900 .
C31 C32 1.3900 .
C32 C33 1.3900 .
C33 C34 1.3900 .
