#------------------------------------------------------------------------------
#$Date: 2025-08-20 14:05:43 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301829 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/75/4067583.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_4067583
loop_
_publ_author_name
'Dzik, Wojciech I.'
'Creusen, Charlotte'
'de Gelder, René'
'Peters, Theo P. J.'
'Smits, Jan M. M.'
'de Bruin, Bas'
_publ_contact_author
;
        Dr. B. de Bruin
        Department of Homogeneous Catalysis
        Van 't Hoff Institute for Molecular Sciences
        University of Amsterdam
        Nieuwe Achtergracht 166
        1018 WV Amsterdam
        The Netherlands
;
_publ_section_title
;
 Carbonyl Complexes of Rhodium with N-Donor Ligands: Factors Determining
 the Formation of Terminal versus Bridging Carbonyls
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1629
_journal_paper_doi               10.1021/om901023n
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_sum            'C66 H76 F18 N12 O10 P3 Rh4'
_chemical_formula_weight         2043.94
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-07-27
_audit_creation_method           'SHELXL, adapted and expanded'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.368(8)
_cell_length_b                   30.368(8)
_cell_length_c                   9.2873(4)
_cell_measurement_reflns_used    618
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.120
_cell_volume                     8565(3)
_computing_data_collection
;
Nonius "Collect" program suite (Nonius, 1999)
;
_computing_data_reduction
;
Nonius "EvalCCD" program suite (Duisenberg, 1998)
;
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF (Beurskens et al., 1996),
PATTY (Beurskens et al., 1987)
;
_diffrn_ambient_temperature      208(2)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.507
_diffrn_measured_fraction_theta_max 0.507
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'area detector φ and ω scan'
_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  0.1218
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            82568
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0.000
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS multiscan (Sheldrick, 1996)'
_exptl_crystal_colour            'translucent yellow-green'
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rather regular rod'
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
The absolute configuration assignment was based on 1686 Friedel pairs
(100% Friedel pair coverage) used to calculate the Flack parameter.
Flack H.D. (1983), Acta Cryst. A39, 876-881.
;
_refine_ls_abs_structure_Flack   0.11(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.231
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0877
_refine_ls_R_factor_obs          0.0877
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0732P)²+193.7336P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2187
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_obs         0.2183
_refine_ls_wR_factor_ref         0.2187
_reflns_number_gt                3738
_reflns_number_observed          3738
_reflns_number_total             3781
_reflns_observed_criterion       >2sigma(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901023n_si_001.cif
_cod_data_source_block           WOJ12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_publ_contact_autor' tag replaced with '_publ_contact_author'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (42
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (84 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C33 H38 F9 N6 O5 P1.50 Rh2'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     1021.97
_cod_database_code               4067583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'-y+1/2, -x, z+3/4'
'x+1/2, -y, -z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'x+1, -y+1/2, -z+5/4'
'y+1, x+1/2, z+5/4'
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_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.55162(3) 0.29198(3) 0.14288(12) 0.0389(3) Uani 1 d .
C1 C 0.5781(4) 0.2448(5) 0.2661(13) 0.037(3) Uani 1 d .
O1 O 0.5990(4) 0.2402(3) 0.3670(15) 0.069(3) Uani 1 d .
C2 C 0.5003(8) 0.2500 0.1250 0.059(6) Uani 1 d S
O2 O 0.4628(4) 0.2500 0.1250 0.065(4) Uani 1 d S
N1 N 0.5222(3) 0.3446(4) 0.0184(12) 0.038(2) Uani 1 d .
N2 N 0.6050(4) 0.3388(4) 0.1743(16) 0.055(3) Uani 1 d .
N3 N 0.5253(4) 0.3338(4) 0.3136(14) 0.049(3) Uani 1 d .
H3 H 0.5138 0.3159 0.3840 0.059 Uiso 1 calc R
C11 C 0.4883(6) 0.3594(5) 0.2488(17) 0.056(4) Uani 1 d .
H11A H 0.4834 0.3861 0.3061 0.067 Uiso 1 calc R
H11B H 0.4613 0.3416 0.2533 0.067 Uiso 1 calc R
C12 C 0.4964(4) 0.3723(4) 0.0959(19) 0.047(3) Uani 1 d .
C13 C 0.4795(5) 0.4099(5) 0.033(2) 0.062(5) Uani 1 d .
H13 H 0.4617 0.4290 0.0867 0.074 Uiso 1 calc R
C14 C 0.4880(5) 0.4188(5) -0.099(3) 0.067(5) Uani 1 d .
H14 H 0.4759 0.4444 -0.1400 0.080 Uiso 1 calc R
C15 C 0.5148(5) 0.3916(5) -0.1853(17) 0.057(4) Uani 1 d .
H15 H 0.5212 0.3977 -0.2823 0.069 Uiso 1 calc R
C16 C 0.5313(4) 0.3540(4) -0.111(2) 0.052(4) Uani 1 d .
H16 H 0.5501 0.3349 -0.1618 0.063 Uiso 1 calc R
C21 C 0.5598(5) 0.3609(5) 0.379(2) 0.065(4) Uani 1 d .
H21A H 0.5699 0.3464 0.4673 0.078 Uiso 1 calc R
H21B H 0.5471 0.3893 0.4061 0.078 Uiso 1 calc R
C22 C 0.5989(5) 0.3690(4) 0.2847(17) 0.049(4) Uani 1 d .
C23 C 0.6274(7) 0.4031(5) 0.290(3) 0.082(7) Uani 1 d .
H23 H 0.6238 0.4248 0.3608 0.098 Uiso 1 calc R
C24 C 0.6619(7) 0.4068(7) 0.194(4) 0.106(10) Uani 1 d .
H24 H 0.6814 0.4307 0.2004 0.128 Uiso 1 calc R
C25 C 0.6675(6) 0.3773(7) 0.094(3) 0.089(7) Uani 1 d .
H25 H 0.6917 0.3794 0.0310 0.107 Uiso 1 calc R
C26 C 0.6382(5) 0.3431(5) 0.080(2) 0.061(4) Uani 1 d .
H26 H 0.6414 0.3227 0.0045 0.074 Uiso 1 calc R
P1 P 1.00663(17) 0.2500 0.1250 0.0500(13) Uani 1 d S
F1 F 1.0579(4) 0.2500 0.1250 0.092(5) Uani 1 d S
F2 F 0.9565(6) 0.2500 0.1250 0.166(12) Uani 1 d S
F3 F 1.0078(6) 0.1981(3) 0.0998(18) 0.121(5) Uani 1 d .
F4 F 1.0063(3) 0.2418(3) 0.2937(12) 0.067(3) Uani 1 d .
P2 P 1.0000 0.5000 0.2500 0.0454(16) Uani 1 d S
F5 F 1.0000 0.5000 0.092(3) 0.166(11) Uani 1 d S
F6 F 1.0244(5) 0.4551(4) 0.248(2) 0.138(6) Uani 1 d .
O31 O 0.3812(5) 0.1288(5) -0.074(3) 0.121(7) Uani 1 d .
C31 C 0.3572(5) 0.1582(7) -0.115(2) 0.071(5) Uani 1 d .
C32 C 0.3120(5) 0.1492(6) -0.141(3) 0.083(6) Uani 1 d .
H32A H 0.3073 0.1176 -0.1420 0.124 Uiso 1 calc R
H32B H 0.3035 0.1615 -0.2330 0.124 Uiso 1 calc R
H32C H 0.2942 0.1622 -0.0651 0.124 Uiso 1 calc R
C33 C 0.3739(6) 0.2035(7) -0.118(4) 0.109(9) Uani 1 d .
H33A H 0.3666 0.2168 -0.2104 0.164 Uiso 1 calc R
H33B H 0.4056 0.2033 -0.1063 0.164 Uiso 1 calc R
H33C H 0.3605 0.2204 -0.0413 0.164 Uiso 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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 '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
_geom_angle_publ_flag
C1 Rh1 C1 82.1(6) . 15_454 y
C1 Rh1 C2 84.6(5) . . y
C1 Rh1 C2 84.2(5) 15_454 . y
C1 Rh1 N1 177.4(5) . . y
C1 Rh1 N1 100.5(5) 15_454 . y
C2 Rh1 N1 96.0(4) . . y
C1 Rh1 N2 95.2(5) . . y
C1 Rh1 N2 99.3(5) 15_454 . y
C2 Rh1 N2 176.5(5) . . y
N1 Rh1 N2 84.1(4) . . y
C1 Rh1 N3 98.6(5) . . y
C1 Rh1 N3 177.5(5) 15_454 . y
C2 Rh1 N3 98.3(5) . . y
N1 Rh1 N3 78.9(4) . . y
N2 Rh1 N3 78.2(5) . . y
C1 Rh1 Rh1 50.5(3) . 15_454 y
C1 Rh1 Rh1 50.0(4) 15_454 15_454 y
C2 Rh1 Rh1 50.5(4) . 15_454 y
N1 Rh1 Rh1 131.5(3) . 15_454 y
N2 Rh1 Rh1 131.7(3) . 15_454 y
N3 Rh1 Rh1 132.1(3) . 15_454 y
O1 C1 Rh1 141.2(11) . . y
O1 C1 Rh1 139.2(12) . 15_454 y
Rh1 C1 Rh1 79.5(4) . 15_454 y
O2 C2 Rh1 140.5(4) . 15_454 y
O2 C2 Rh1 140.5(4) . . y
Rh1 C2 Rh1 79.1(8) 15_454 . y
C16 N1 C12 119.3(12) . . y
C16 N1 Rh1 125.7(9) . . y
C12 N1 Rh1 114.4(10) . . y
C26 N2 C22 121.1(12) . . y
C26 N2 Rh1 122.4(11) . . y
C22 N2 Rh1 115.6(10) . . y
C21 N3 C11 114.6(11) . . y
C21 N3 Rh1 111.4(9) . . y
C11 N3 Rh1 106.6(8) . . y
N3 C11 C12 113.2(12) . . y
N1 C12 C13 120.1(16) . . y
N1 C12 C11 115.9(12) . . y
C13 C12 C11 124.0(14) . . y
C14 C13 C12 120.5(17) . . y
C13 C14 C15 122.3(17) . . y
C14 C15 C16 113.6(15) . . y
N1 C16 C15 124.3(14) . . y
N3 C21 C22 114.9(13) . . y
C23 C22 N2 116.6(17) . . y
C23 C22 C21 128.1(16) . . y
N2 C22 C21 115.3(12) . . y
C22 C23 C24 122(2) . . y
C25 C24 C23 120.3(18) . . y
C24 C25 C26 120(2) . . y
N2 C26 C25 120.0(18) . . y
F2 P1 F1 180.0 . . ?
F2 P1 F4 89.6(4) . . y
F1 P1 F4 90.4(4) . . y
F2 P1 F4 89.6(4) . 15_454 y
F1 P1 F4 90.4(4) . 15_454 y
F4 P1 F4 179.2(8) . 15_454 y
F2 P1 F3 91.3(6) . . y
F1 P1 F3 88.7(6) . . y
F4 P1 F3 89.4(7) . . y
F4 P1 F3 90.6(7) 15_454 . y
F2 P1 F3 91.3(6) . 15_454 y
F1 P1 F3 88.7(6) . 15_454 y
F4 P1 F3 90.6(7) . 15_454 y
F4 P1 F3 89.4(7) 15_454 15_454 y
F3 P1 F3 177.3(13) . 15_454 y
F5 P2 F5 179.995(7) . 10_565 y
F5 P2 F6 89.3(7) . 3_765 y
F5 P2 F6 90.7(7) 10_565 3_765 y
F5 P2 F6 90.7(7) . 12_645 y
F5 P2 F6 89.3(7) 10_565 12_645 y
F6 P2 F6 90.01(2) 3_765 12_645 y
F5 P2 F6 89.3(7) . . y
F5 P2 F6 90.7(7) 10_565 . y
F6 P2 F6 178.5(14) 3_765 . y
F6 P2 F6 90.01(2) 12_645 . y
F5 P2 F6 90.7(7) . 10_565 y
F5 P2 F6 89.3(7) 10_565 10_565 y
F6 P2 F6 90.01(2) 3_765 10_565 y
F6 P2 F6 178.5(14) 12_645 10_565 y
F6 P2 F6 90.006(17) . 10_565 y
O31 C31 C32 119.5(19) . . y
O31 C31 C33 119.4(18) . . y
C32 C31 C33 120.7(18) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 2.004(14) . y
Rh1 C1 2.019(12) 15_454 y
Rh1 C2 2.019(18) . y
Rh1 N1 2.165(11) . y
Rh1 N2 2.176(12) . y
Rh1 N3 2.184(12) . y
Rh1 Rh1 2.5710(18) 15_454 y
C1 O1 1.140(16) . y
C1 Rh1 2.019(12) 15_454 y
C2 O2 1.14(2) . y
C2 Rh1 2.019(18) 15_454 y
N1 C16 1.27(2) . y
N1 C12 1.356(17) . y
N2 C26 1.34(2) . y
N2 C22 1.390(19) . y
N3 C21 1.46(2) . y
N3 C11 1.49(2) . y
C11 C12 1.49(2) . y
C12 C13 1.38(2) . y
C13 C14 1.28(3) . y
C14 C15 1.41(2) . y
C15 C16 1.42(2) . y
C21 C22 1.50(2) . y
C22 C23 1.35(2) . y
C23 C24 1.38(3) . y
C24 C25 1.30(3) . y
C25 C26 1.37(2) . y
P1 F2 1.524(18) . y
P1 F1 1.558(14) . y
P1 F4 1.586(11) . y
P1 F4 1.586(11) 15_454 y
P1 F3 1.595(11) . y
P1 F3 1.595(11) 15_454 y
P2 F5 1.47(2) . y
P2 F5 1.47(2) 10_565 y
P2 F6 1.552(12) 3_765 y
P2 F6 1.552(12) 12_645 y
P2 F6 1.553(12) . y
P2 F6 1.553(12) 10_565 y
O31 C31 1.21(2) . y
C31 C32 1.42(2) . y
C31 C33 1.47(3) . y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168332058
