#------------------------------------------------------------------------------
#$Date: 2016-03-21 13:12:26 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178693 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/04/4080407.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_4080407
loop_
_publ_author_name
'Shuster, Vladimir'
'Gambarotta, Sandro'
'Nikiforov, Grigory B.'
'Budzelaar, Peter H. M.'
_publ_section_title
;
 Heterometallic Aluminum--Chromium Phenazine and Thiophenazine Complexes.
 Formation of a Tetranuclear Chromium(I) Sandwich Complex
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2329
_journal_paper_doi               10.1021/om3012097
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C32 H36 Al2 Cl2 Cr N2 S2'
_chemical_formula_weight         689.61
_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                106.479(2)
_cell_angle_beta                 95.036(2)
_cell_angle_gamma                107.048(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3503(13)
_cell_length_b                   9.9256(14)
_cell_length_c                   10.0618(14)
_cell_measurement_reflns_used    6660
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.15
_cell_volume                     841.1(2)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7840
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.9023
_exptl_absorpt_correction_T_min  0.8727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            blue_purple
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0958P)²+0.6534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                2492
_reflns_number_total             2807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3012097_si_001.cif
_cod_data_source_block           sg3914
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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      P-1
_cod_database_code               4080407
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
Cr1 Cr 0.0000 0.0000 1.0000 0.0263(2) Uani 1 2 d S
Cl1 Cl 0.08982(10) 0.08879(8) 0.81728(8) 0.0395(3) Uani 1 1 d .
S1 S 0.07621(9) 0.51909(9) 1.33735(8) 0.0375(2) Uani 1 1 d .
Al1 Al 0.05008(10) -0.15880(9) 0.69459(9) 0.0288(3) Uani 1 1 d .
N1 N 0.0280(3) 0.2149(3) 1.1424(2) 0.0261(5) Uani 1 1 d .
C1 C 0.2254(3) 0.4536(3) 1.2854(3) 0.0307(6) Uani 1 1 d .
C2 C 0.3759(4) 0.5416(4) 1.3385(3) 0.0399(8) Uani 1 1 d .
H2A H 0.3999 0.6397 1.4025 0.048 Uiso 1 1 calc R
C3 C 0.4909(4) 0.4878(4) 1.2990(4) 0.0458(8) Uani 1 1 d .
H3A H 0.5942 0.5485 1.3359 0.055 Uiso 1 1 calc R
C4 C 0.4563(4) 0.3451(4) 1.2054(4) 0.0421(8) Uani 1 1 d .
H4A H 0.5356 0.3076 1.1781 0.051 Uiso 1 1 calc R
C5 C 0.3048(4) 0.2569(4) 1.1516(3) 0.0353(7) Uani 1 1 d .
H5A H 0.2814 0.1593 1.0871 0.042 Uiso 1 1 calc R
C6 C 0.1878(3) 0.3091(3) 1.1907(3) 0.0277(6) Uani 1 1 d .
C7 C -0.0529(3) 0.4360(3) 1.1745(3) 0.0291(6) Uani 1 1 d .
C8 C -0.1433(3) 0.5102(3) 1.1323(4) 0.0351(7) Uani 1 1 d .
H8A H -0.1306 0.6096 1.1872 0.042 Uiso 1 1 calc R
C9 C -0.2521(4) 0.4397(4) 1.0102(4) 0.0394(8) Uani 1 1 d .
H9A H -0.3161 0.4895 0.9823 0.047 Uiso 1 1 calc R
C10 C -0.2676(4) 0.2964(4) 0.9286(4) 0.0381(7) Uani 1 1 d .
H10A H -0.3423 0.2478 0.8445 0.046 Uiso 1 1 calc R
C11 C -0.1737(3) 0.2232(3) 0.9697(3) 0.0331(7) Uani 1 1 d .
H11A H -0.1842 0.1252 0.9126 0.040 Uiso 1 1 calc R
C12 C -0.0655(3) 0.2917(3) 1.0926(3) 0.0267(6) Uani 1 1 d .
C13 C 0.2551(4) -0.1677(4) 0.6782(4) 0.0413(8) Uani 1 1 d .
H13A H 0.2570 -0.2644 0.6859 0.050 Uiso 1 1 calc R
H13B H 0.2707 -0.1685 0.5819 0.050 Uiso 1 1 calc R
C14 C 0.3893(5) -0.0474(5) 0.7808(6) 0.0754(14) Uani 1 1 d .
H14A H 0.4833 -0.0663 0.7595 0.113 Uiso 1 1 calc R
H14B H 0.3794 -0.0472 0.8770 0.113 Uiso 1 1 calc R
H14C H 0.3927 0.0495 0.7728 0.113 Uiso 1 1 calc R
C15 C -0.1049(4) -0.2058(4) 0.5287(3) 0.0408(8) Uani 1 1 d .
H15A H -0.0510 -0.1767 0.4555 0.049 Uiso 1 1 calc R
H15B H -0.1533 -0.3155 0.4923 0.049 Uiso 1 1 calc R
C16 C -0.2327(5) -0.1386(5) 0.5407(4) 0.0576(10) Uani 1 1 d .
H16A H -0.2992 -0.1732 0.4483 0.086 Uiso 1 1 calc R
H16B H -0.1888 -0.0296 0.5727 0.086 Uiso 1 1 calc R
H16C H -0.2922 -0.1698 0.6087 0.086 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_3
N1 Cr1 N1 180.0 . 2_557
N1 Cr1 Cl1 94.95(7) . .
N1 Cr1 Cl1 85.05(7) 2_557 .
N1 Cr1 Cl1 85.05(7) . 2_557
N1 Cr1 Cl1 94.95(7) 2_557 2_557
Cl1 Cr1 Cl1 180.0 . 2_557
Al1 Cl1 Cr1 85.31(3) . .
C1 S1 C7 98.54(14) . .
C15 Al1 C13 122.00(15) . .
C15 Al1 N1 115.64(12) . 2_557
C13 Al1 N1 113.97(13) . 2_557
C15 Al1 Cl1 104.18(11) . .
C13 Al1 Cl1 104.46(11) . .
N1 Al1 Cl1 89.39(7) 2_557 .
C12 N1 C6 112.1(2) . .
C12 N1 Al1 108.47(17) . 2_557
C6 N1 Al1 108.15(17) . 2_557
C12 N1 Cr1 114.33(17) . .
C6 N1 Cr1 112.70(17) . .
Al1 N1 Cr1 100.22(10) 2_557 .
C2 C1 C6 120.7(3) . .
C2 C1 S1 120.9(2) . .
C6 C1 S1 118.4(2) . .
C3 C2 C1 120.2(3) . .
C2 C3 C4 120.1(3) . .
C5 C4 C3 119.6(3) . .
C6 C5 C4 121.0(3) . .
C5 C6 C1 118.4(3) . .
C5 C6 N1 121.8(3) . .
C1 C6 N1 119.7(3) . .
C8 C7 C12 121.1(3) . .
C8 C7 S1 120.5(2) . .
C12 C7 S1 118.4(2) . .
C9 C8 C7 120.0(3) . .
C10 C9 C8 119.8(3) . .
C9 C10 C11 120.1(3) . .
C12 C11 C10 120.8(3) . .
C11 C12 C7 118.3(3) . .
C11 C12 N1 122.0(3) . .
C7 C12 N1 119.6(2) . .
C14 C13 Al1 118.7(3) . .
C16 C15 Al1 120.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N1 2.131(2) .
Cr1 N1 2.131(2) 2_557
Cr1 Cl1 2.3704(8) .
Cr1 Cl1 2.3704(8) 2_557
Cl1 Al1 2.3161(12) .
S1 C1 1.763(3) .
S1 C7 1.768(3) .
Al1 C15 1.959(3) .
Al1 C13 1.964(3) .
Al1 N1 2.006(3) 2_557
N1 C12 1.459(4) .
N1 C6 1.462(4) .
N1 Al1 2.006(3) 2_557
C1 C2 1.383(4) .
C1 C6 1.399(4) .
C2 C3 1.375(5) .
C3 C4 1.385(5) .
C4 C5 1.391(5) .
C5 C6 1.382(4) .
C7 C8 1.385(4) .
C7 C12 1.400(4) .
C8 C9 1.382(5) .
C9 C10 1.383(5) .
C10 C11 1.397(4) .
C11 C12 1.383(4) .
C13 C14 1.504(6) .
C15 C16 1.529(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Cr1 Cl1 Al1 178.72(6) . .
N1 Cr1 Cl1 Al1 -1.28(6) 2_557 .
Cl1 Cr1 Cl1 Al1 58(19) 2_557 .
Cr1 Cl1 Al1 C15 117.70(11) . .
Cr1 Cl1 Al1 C13 -113.27(12) . .
Cr1 Cl1 Al1 N1 1.36(7) . 2_557
N1 Cr1 N1 C12 -76(32) 2_557 .
Cl1 Cr1 N1 C12 62.73(18) . .
Cl1 Cr1 N1 C12 -117.27(18) 2_557 .
N1 Cr1 N1 C6 155(32) 2_557 .
Cl1 Cr1 N1 C6 -66.76(18) . .
Cl1 Cr1 N1 C6 113.24(18) 2_557 .
N1 Cr1 N1 Al1 40(32) 2_557 2_557
Cl1 Cr1 N1 Al1 178.50(7) . 2_557
Cl1 Cr1 N1 Al1 -1.50(7) 2_557 2_557
C7 S1 C1 C2 143.6(3) . .
C7 S1 C1 C6 -37.4(3) . .
C6 C1 C2 C3 -0.2(5) . .
S1 C1 C2 C3 178.7(3) . .
C1 C2 C3 C4 0.2(5) . .
C2 C3 C4 C5 0.1(5) . .
C3 C4 C5 C6 -0.4(5) . .
C4 C5 C6 C1 0.3(5) . .
C4 C5 C6 N1 -176.0(3) . .
C2 C1 C6 C5 0.0(4) . .
S1 C1 C6 C5 -179.0(2) . .
C2 C1 C6 N1 176.4(3) . .
S1 C1 C6 N1 -2.6(4) . .
C12 N1 C6 C5 -134.0(3) . .
Al1 N1 C6 C5 106.5(3) 2_557 .
Cr1 N1 C6 C5 -3.4(3) . .
C12 N1 C6 C1 49.7(3) . .
Al1 N1 C6 C1 -69.8(3) 2_557 .
Cr1 N1 C6 C1 -179.7(2) . .
C1 S1 C7 C8 -143.4(3) . .
C1 S1 C7 C12 39.1(3) . .
C12 C7 C8 C9 2.4(5) . .
S1 C7 C8 C9 -175.0(2) . .
C7 C8 C9 C10 -1.6(5) . .
C8 C9 C10 C11 0.1(5) . .
C9 C10 C11 C12 0.7(5) . .
C10 C11 C12 C7 0.1(4) . .
C10 C11 C12 N1 176.4(3) . .
C8 C7 C12 C11 -1.6(4) . .
S1 C7 C12 C11 175.8(2) . .
C8 C7 C12 N1 -178.0(3) . .
S1 C7 C12 N1 -0.6(4) . .
C6 N1 C12 C11 135.9(3) . .
Al1 N1 C12 C11 -104.7(3) 2_557 .
Cr1 N1 C12 C11 6.1(3) . .
C6 N1 C12 C7 -47.8(3) . .
Al1 N1 C12 C7 71.5(3) 2_557 .
Cr1 N1 C12 C7 -177.6(2) . .
C15 Al1 C13 C14 139.0(3) . .
N1 Al1 C13 C14 -74.3(4) 2_557 .
Cl1 Al1 C13 C14 21.6(4) . .
C13 Al1 C15 C16 -154.1(3) . .
N1 Al1 C15 C16 59.7(3) 2_557 .
Cl1 Al1 C15 C16 -36.6(3) . .
