#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:05:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178594 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/05/4070571.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_4070571
loop_
_publ_author_name
'Das, Atanu Kumar'
'Bulak, Ece'
'Sarkar, Biprajit'
'Lissner, Falk'
'Schleid, Thomas'
'Niemeyer, Mark'
'Fiedler, Jan'
'Kaim, Wolfgang'
_publ_section_title
;
 Structures and Redox Properties of Metal Complexes of the
 Electron-Deficient Diphosphine Chelate LigandR,R-QuinoxP
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              218
_journal_paper_doi               10.1021/om700755y
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C21 H28 Cl N2 O3 P2 Re'
_chemical_formula_weight         640.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 104.375(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.692(4)
_cell_length_b                   11.993(2)
_cell_length_c                   10.4390(15)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     2752.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3314
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.650
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3314
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0278
_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)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3056
_reflns_number_total             3314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700755y-file003.cif
_cod_data_source_block           da02
_cod_original_cell_volume        2751.9(8)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4070571
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Re Re 0.730412(9) 0.23310(5) 0.73700(2) 0.02077(7) Uani 1 1 d .
Cl Cl 0.73553(9) 0.20837(14) 0.97761(19) 0.0339(5) Uani 1 1 d .
P1 P 0.64141(9) 0.10562(17) 0.6895(2) 0.0210(4) Uani 1 1 d .
P2 P 0.65245(8) 0.37263(16) 0.7492(2) 0.0181(4) Uani 1 1 d .
N1 N 0.5336(4) 0.1183(8) 0.7676(7) 0.0226(17) Uani 1 1 d .
N2 N 0.5406(4) 0.3521(8) 0.8031(8) 0.0232(17) Uani 1 1 d .
C1 C 0.5810(5) 0.1783(9) 0.7475(10) 0.019(2) Uani 1 1 d .
C2 C 0.4902(6) 0.1758(10) 0.8062(10) 0.023(2) Uani 1 1 d .
C3 C 0.4385(5) 0.1145(10) 0.8273(11) 0.026(2) Uani 1 1 d .
H3A H 0.4370 0.0371 0.8211 0.046(11) Uiso 1 1 calc R
C4 C 0.3919(6) 0.1738(12) 0.8569(11) 0.032(3) Uani 1 1 d .
H4A H 0.3587 0.1354 0.8723 0.046(11) Uiso 1 1 calc R
C5 C 0.3927(6) 0.2900(12) 0.8646(11) 0.031(3) Uani 1 1 d .
H5A H 0.3591 0.3281 0.8785 0.046(11) Uiso 1 1 calc R
C6 C 0.4422(6) 0.3473(10) 0.8517(11) 0.030(3) Uani 1 1 d .
H6A H 0.4439 0.4241 0.8644 0.046(11) Uiso 1 1 calc R
C7 C 0.4909(5) 0.2922(10) 0.8195(10) 0.020(2) Uani 1 1 d .
C8 C 0.5842(5) 0.2973(10) 0.7689(10) 0.020(2) Uani 1 1 d .
C9 C 0.6715(3) 0.4607(7) 0.8957(7) 0.0271(15) Uani 1 1 d .
H9A H 0.6348 0.4848 0.9174 0.049(6) Uiso 1 1 calc R
H9B H 0.6939 0.5246 0.8786 0.049(6) Uiso 1 1 calc R
H9C H 0.6959 0.4192 0.9684 0.049(6) Uiso 1 1 calc R
C10 C 0.6242(3) 0.4731(6) 0.6106(7) 0.0273(15) Uani 1 1 d .
C11 C 0.5905(5) 0.4111(9) 0.4875(9) 0.036(2) Uani 1 1 d .
H11A H 0.5791 0.4624 0.4150 0.049(6) Uiso 1 1 calc R
H11B H 0.5547 0.3771 0.5033 0.049(6) Uiso 1 1 calc R
H11C H 0.6164 0.3544 0.4664 0.049(6) Uiso 1 1 calc R
C12 C 0.5808(6) 0.5607(9) 0.6457(11) 0.035(3) Uani 1 1 d .
H12A H 0.5628 0.6042 0.5687 0.049(6) Uiso 1 1 calc R
H12B H 0.6032 0.6088 0.7142 0.049(6) Uiso 1 1 calc R
H12C H 0.5493 0.5236 0.6761 0.049(6) Uiso 1 1 calc R
C13 C 0.6811(4) 0.5338(7) 0.5841(9) 0.0369(19) Uani 1 1 d .
H13A H 0.6685 0.5820 0.5089 0.049(6) Uiso 1 1 calc R
H13B H 0.7092 0.4794 0.5669 0.049(6) Uiso 1 1 calc R
H13C H 0.7005 0.5771 0.6603 0.049(6) Uiso 1 1 calc R
C14 C 0.6059(4) 0.0929(8) 0.5112(8) 0.031(2) Uani 1 1 d .
H14A H 0.5651 0.0653 0.4984 0.049(6) Uiso 1 1 calc R
H14B H 0.6291 0.0421 0.4721 0.049(6) Uiso 1 1 calc R
H14C H 0.6049 0.1647 0.4700 0.049(6) Uiso 1 1 calc R
C15 C 0.6436(4) -0.0410(6) 0.7496(8) 0.0282(15) Uani 1 1 d .
C16 C 0.6497(5) -0.0457(8) 0.9000(8) 0.0385(19) Uani 1 1 d .
H16A H 0.6597 -0.1203 0.9312 0.049(6) Uiso 1 1 calc R
H16B H 0.6119 -0.0240 0.9182 0.049(6) Uiso 1 1 calc R
H16C H 0.6813 0.0043 0.9441 0.049(6) Uiso 1 1 calc R
C17 C 0.5875(7) -0.1084(11) 0.6788(15) 0.049(3) Uani 1 1 d .
H17A H 0.5922 -0.1845 0.7083 0.049(6) Uiso 1 1 calc R
H17B H 0.5833 -0.1058 0.5851 0.049(6) Uiso 1 1 calc R
H17C H 0.5518 -0.0772 0.6989 0.049(6) Uiso 1 1 calc R
C18 C 0.7004(5) -0.0961(7) 0.7212(11) 0.052(3) Uani 1 1 d .
H18A H 0.7021 -0.1730 0.7475 0.049(6) Uiso 1 1 calc R
H18B H 0.7362 -0.0583 0.7701 0.049(6) Uiso 1 1 calc R
H18C H 0.6982 -0.0914 0.6284 0.049(6) Uiso 1 1 calc R
C19 C 0.7242(3) 0.2438(14) 0.5488(7) 0.0315(16) Uani 1 1 d .
O19 O 0.7210(3) 0.2475(11) 0.4395(5) 0.0463(17) Uani 1 1 d .
C20 C 0.7916(6) 0.3493(12) 0.7657(12) 0.036(3) Uani 1 1 d .
O20 O 0.8251(5) 0.4230(9) 0.7729(11) 0.049(3) Uani 1 1 d .
C21 C 0.7941(7) 0.1183(11) 0.7591(12) 0.031(3) Uani 1 1 d .
O21 O 0.8331(6) 0.0563(10) 0.7723(12) 0.054(3) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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'
Re Re -1.0185 7.2310 '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
C20 Re C19 88.7(5)
C20 Re C21 90.4(3)
C19 Re C21 91.8(5)
C20 Re P2 90.0(4)
C19 Re P2 97.8(4)
C21 Re P2 170.4(4)
C20 Re P1 171.9(4)
C19 Re P1 89.3(3)
C21 Re P1 97.5(4)
P2 Re P1 82.50(6)
C20 Re Cl 94.4(4)
C19 Re Cl 176.7(5)
C21 Re Cl 87.1(4)
P2 Re Cl 83.30(7)
P1 Re Cl 87.71(7)
C14 P1 C1 101.3(5)
C14 P1 C15 103.3(4)
C1 P1 C15 107.1(4)
C14 P1 Re 112.5(3)
C1 P1 Re 106.1(3)
C15 P1 Re 124.1(3)
C9 P2 C8 102.8(4)
C9 P2 C10 103.9(4)
C8 P2 C10 105.4(4)
C9 P2 Re 114.5(3)
C8 P2 Re 107.8(4)
C10 P2 Re 120.7(2)
C2 N1 C1 116.4(10)
C8 N2 C7 117.9(10)
N1 C1 C8 120.9(12)
N1 C1 P1 118.9(8)
C8 C1 P1 120.2(10)
N1 C2 C7 123.2(13)
N1 C2 C3 117.9(11)
C7 C2 C3 118.8(13)
C4 C3 C2 118.1(11)
C3 C4 C5 122.0(15)
C6 C5 C4 120.0(15)
C5 C6 C7 120.7(12)
N2 C7 C6 120.1(11)
N2 C7 C2 119.6(13)
C6 C7 C2 120.2(13)
N2 C8 C1 121.7(12)
N2 C8 P2 119.7(9)
C1 C8 P2 118.6(11)
C11 C10 C12 108.5(8)
C11 C10 C13 110.1(7)
C12 C10 C13 109.2(8)
C11 C10 P2 110.1(6)
C12 C10 P2 111.7(6)
C13 C10 P2 107.3(5)
C17 C15 C18 108.4(9)
C17 C15 C16 108.9(9)
C18 C15 C16 108.2(7)
C17 C15 P1 112.7(7)
C18 C15 P1 107.1(6)
C16 C15 P1 111.4(6)
O19 C19 Re 178.4(15)
O20 C20 Re 174.0(11)
O21 C21 Re 176.4(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re C20 1.937(15)
Re C19 1.939(7)
Re C21 1.968(14)
Re P2 2.461(2)
Re P1 2.483(2)
Re Cl 2.5031(19)
P1 C14 1.842(9)
P1 C1 1.848(12)
P1 C15 1.864(8)
P2 C9 1.820(8)
P2 C8 1.847(11)
P2 C10 1.870(7)
N1 C2 1.344(15)
N1 C1 1.353(13)
N2 C8 1.309(14)
N2 C7 1.383(14)
C1 C8 1.444(9)
C2 C7 1.403(9)
C2 C3 1.445(16)
C3 C4 1.373(18)
C4 C5 1.396(11)
C5 C6 1.352(18)
C6 C7 1.398(16)
C10 C11 1.517(12)
C10 C12 1.546(14)
C10 C13 1.564(10)
C15 C17 1.535(16)
C15 C18 1.540(11)
C15 C16 1.543(11)
C19 O19 1.126(8)
C20 O20 1.156(18)
C21 O21 1.138(18)
