#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:28:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178566 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/75/4067584.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_4067584
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_formula_sum            'C24 H32 F6 N3 O P Rh'
_chemical_formula_weight         626.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3568(9)
_cell_length_b                   21.675(2)
_cell_length_c                   13.0980(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13.159
_cell_measurement_theta_min      8.901
_cell_volume                     2653.8(5)
_computing_data_collection
;
CAD4 EXPRESS (Enraf-Nonius, 1994)
;
_computing_data_reduction
;
local programs (Smits et al., 1988),
profile analysis (Lehman & Larsen, 1974, Grant & Gabe, 1978),
EMPABS (North et al., 1968)
;
_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      298(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       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  0.1070
_diffrn_reflns_av_sigmaI/netI    0.1398
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9730
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        2.658
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular chunk'
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4648
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0688
_refine_ls_R_factor_obs          0.0688
_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)+(0.0687P)²+0.6537P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1683
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_obs         0.1375
_refine_ls_wR_factor_ref         0.1683
_reflns_number_gt                2478
_reflns_number_observed          2478
_reflns_number_total             4648
_reflns_observed_criterion       >2sigma(I)
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901023n_si_001.cif
_cod_data_source_block           DUOGAL
_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 (43
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 (87 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2653.7(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067584
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.26910(8) 0.15205(3) 0.03433(5) 0.0356(2) Uani 1 d . . .
N1 N 0.4616(8) 0.2059(3) 0.0586(5) 0.0349(17) Uani 1 d . . .
N2 N 0.2866(7) 0.1455(3) 0.1957(5) 0.0329(16) Uani 1 d . . .
N3 N 0.4547(8) 0.0763(3) 0.0652(5) 0.0391(18) Uani 1 d . . .
C11 C 0.5919(10) 0.1084(4) 0.0595(7) 0.044(2) Uani 1 d . . .
H11A H 0.6256 0.1042 -0.0091 0.053 Uiso 1 calc R . .
H11B H 0.6614 0.0887 0.1060 0.053 Uiso 1 calc R . .
C12 C 0.5833(11) 0.1763(4) 0.0861(7) 0.044(2) Uani 1 d . . .
C13 C 0.6993(10) 0.2074(5) 0.1265(6) 0.047(2) Uani 1 d . . .
H13 H 0.7823 0.1859 0.1455 0.056 Uiso 1 calc R . .
C14 C 0.6944(12) 0.2704(5) 0.1393(7) 0.060(3) Uani 1 d . . .
H14 H 0.7727 0.2921 0.1670 0.071 Uiso 1 calc R . .
C15 C 0.5693(12) 0.3003(5) 0.1097(7) 0.054(3) Uani 1 d . . .
H15 H 0.5628 0.3430 0.1157 0.064 Uiso 1 calc R . .
C16 C 0.4561(10) 0.2675(4) 0.0718(6) 0.043(2) Uani 1 d . . .
H16 H 0.3714 0.2882 0.0543 0.051 Uiso 1 calc R . .
C21 C 0.4285(10) 0.0537(4) 0.1701(6) 0.044(2) Uani 1 d . . .
H21A H 0.5179 0.0385 0.2008 0.053 Uiso 1 calc R . .
H21B H 0.3624 0.0193 0.1650 0.053 Uiso 1 calc R . .
C22 C 0.3693(9) 0.1012(4) 0.2392(6) 0.036(2) Uani 1 d . . .
C23 C 0.3934(10) 0.0984(4) 0.3430(7) 0.046(2) Uani 1 d . . .
H23 H 0.4508 0.0673 0.3716 0.055 Uiso 1 calc R . .
C24 C 0.3330(11) 0.1416(5) 0.4052(7) 0.056(3) Uani 1 d . . .
H24 H 0.3498 0.1404 0.4757 0.068 Uiso 1 calc R . .
C25 C 0.2469(10) 0.1866(5) 0.3604(7) 0.051(3) Uani 1 d . . .
H25 H 0.2018 0.2155 0.4006 0.061 Uiso 1 calc R . .
C26 C 0.2285(10) 0.1885(4) 0.2558(7) 0.043(2) Uani 1 d . . .
H26 H 0.1745 0.2201 0.2256 0.051 Uiso 1 calc R . .
C31 C 0.4465(10) 0.0258(4) -0.0096(6) 0.043(2) Uani 1 d . . .
H31A H 0.4605 0.0428 -0.0769 0.051 Uiso 1 calc R . .
H31B H 0.3509 0.0084 -0.0104 0.051 Uiso 1 calc R . .
C1 C 0.2265(10) 0.2031(4) -0.1011(6) 0.046(2) Uani 1 d . . .
H1 H 0.3057 0.2304 -0.1179 0.055 Uiso 1 calc R . .
C2 C 0.2503(12) 0.1425(4) -0.1271(7) 0.056(3) Uani 1 d . . .
H2 H 0.3415 0.1355 -0.1592 0.067 Uiso 1 calc R . .
C3 C 0.1311(17) 0.0981(6) -0.1632(9) 0.104(5) Uani 1 d . . .
H3A H 0.0588 0.1208 -0.2030 0.125 Uiso 1 calc R . .
H3B H 0.1706 0.0671 -0.2072 0.125 Uiso 1 calc R . .
C4 C 0.0632(15) 0.0673(6) -0.0769(10) 0.094(4) Uani 1 d . . .
H4A H 0.1014 0.0258 -0.0702 0.113 Uiso 1 calc R . .
H4B H -0.0386 0.0638 -0.0931 0.113 Uiso 1 calc R . .
C5 C 0.0841(12) 0.0993(6) 0.0234(9) 0.076(4) Uani 1 d . . .
H5 H 0.0714 0.0725 0.0825 0.091 Uiso 1 calc R . .
C6 C 0.0465(10) 0.1631(6) 0.0409(8) 0.069(3) Uani 1 d . . .
H6 H 0.0141 0.1713 0.1097 0.082 Uiso 1 calc R . .
C7 C -0.0232(10) 0.2025(6) -0.0400(8) 0.069(3) Uani 1 d . . .
H7A H -0.0843 0.2325 -0.0085 0.083 Uiso 1 calc R . .
H7B H -0.0829 0.1770 -0.0853 0.083 Uiso 1 calc R . .
C8 C 0.0855(12) 0.2359(5) -0.1017(8) 0.074(4) Uani 1 d . . .
H8A H 0.0483 0.2400 -0.1716 0.089 Uiso 1 calc R . .
H8B H 0.0999 0.2771 -0.0740 0.089 Uiso 1 calc R . .
P1 P 0.6357(4) 0.11560(15) 0.6862(3) 0.0748(10) Uani 1 d . . .
F1 F 0.6276(12) 0.0983(5) 0.7969(6) 0.161(4) Uani 1 d . . .
F2 F 0.6553(17) 0.1272(6) 0.5710(8) 0.211(6) Uani 1 d . . .
F3 F 0.7723(10) 0.1516(5) 0.7089(8) 0.166(5) Uani 1 d . . .
F4 F 0.7055(18) 0.0548(5) 0.6717(10) 0.245(8) Uani 1 d . . .
F5 F 0.4913(14) 0.0860(6) 0.6740(12) 0.228(7) Uani 1 d . . .
F6 F 0.5582(13) 0.1755(4) 0.6887(15) 0.248(8) Uani 1 d . . .
C41 C 0.8423(18) 0.0501(7) 0.3395(11) 0.111(6) Uani 1 d D . .
O41 O 0.7811(16) 0.0596(6) 0.2627(10) 0.175(6) Uani 1 d . . .
C42 C 0.788(2) 0.0015(8) 0.4151(13) 0.150(7) Uani 1 d D . .
H42A H 0.7016 -0.0167 0.3874 0.225 Uiso 1 calc R . .
H42B H 0.7702 0.0211 0.4790 0.225 Uiso 1 calc R . .
H42C H 0.8597 -0.0299 0.4259 0.225 Uiso 1 calc R . .
C43A C 0.894(5) 0.1058(14) 0.399(3) 0.102(17) Uani 0.36(3) d PD A 1
H43A H 0.9111 0.0946 0.4696 0.153 Uiso 0.36(3) calc PR A 1
H43B H 0.8218 0.1374 0.3945 0.153 Uiso 0.36(3) calc PR A 1
H43C H 0.9803 0.1209 0.3719 0.153 Uiso 0.36(3) calc PR A 1
C43B C 1.005(2) 0.0474(19) 0.344(2) 0.21(3) Uani 0.64(3) d PD A 2
H43D H 1.0357 0.0051 0.3422 0.311 Uiso 0.64(3) calc PR A 2
H43E H 1.0414 0.0660 0.4069 0.311 Uiso 0.64(3) calc PR A 2
H43F H 1.0415 0.0693 0.2874 0.311 Uiso 0.64(3) 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'
N N 0.0061 0.0033 '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'
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'
O O 0.0106 0.0060 '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_3
_geom_angle_publ_flag
C5 Rh1 C6 40.5(4) . y
C5 Rh1 C1 96.0(4) . y
C6 Rh1 C1 79.9(4) . y
C5 Rh1 N2 93.4(4) . y
C6 Rh1 N2 90.0(3) . y
C1 Rh1 N2 151.2(3) . y
C5 Rh1 C2 81.1(5) . y
C6 Rh1 C2 90.7(4) . y
C1 Rh1 C2 38.0(3) . y
N2 Rh1 C2 170.6(3) . y
C5 Rh1 N1 175.5(4) . y
C6 Rh1 N1 139.0(4) . y
C1 Rh1 N1 88.0(3) . y
N2 Rh1 N1 82.1(2) . y
C2 Rh1 N1 103.4(4) . y
C5 Rh1 N3 103.2(4) . y
C6 Rh1 N3 141.1(4) . y
C1 Rh1 N3 127.2(3) . y
N2 Rh1 N3 76.3(2) . y
C2 Rh1 N3 97.3(3) . y
N1 Rh1 N3 75.7(3) . y
C12 N1 C16 118.4(8) . y
C12 N1 Rh1 118.3(6) . y
C16 N1 Rh1 121.2(6) . y
C22 N2 C26 119.1(7) . y
C22 N2 Rh1 119.2(5) . y
C26 N2 Rh1 121.4(6) . y
C11 N3 C31 109.9(7) . y
C11 N3 C21 112.5(7) . y
C31 N3 C21 111.4(6) . y
C11 N3 Rh1 107.1(5) . y
C31 N3 Rh1 112.3(5) . y
C21 N3 Rh1 103.4(5) . y
N3 C11 C12 113.2(7) . y
N1 C12 C13 121.2(9) . y
N1 C12 C11 117.1(9) . y
C13 C12 C11 121.3(9) . y
C12 C13 C14 120.5(10) . y
C13 C14 C15 117.6(10) . y
C16 C15 C14 119.9(9) . y
N1 C16 C15 122.3(9) . y
N3 C21 C22 114.4(6) . y
N2 C22 C23 121.2(8) . y
N2 C22 C21 117.3(7) . y
C23 C22 C21 121.5(8) . y
C22 C23 C24 120.2(9) . y
C23 C24 C25 118.4(9) . y
C26 C25 C24 119.3(9) . y
N2 C26 C25 121.7(8) . y
N3 C31 C31 115.1(9) 3_655 y
C2 C1 C8 127.1(10) . y
C2 C1 Rh1 71.4(5) . y
C8 C1 Rh1 112.7(6) . y
C1 C2 C3 123.5(10) . y
C1 C2 Rh1 70.6(5) . y
C3 C2 Rh1 113.3(7) . y
C4 C3 C2 112.3(9) . y
C3 C4 C5 114.7(10) . y
C6 C5 C4 124.1(11) . y
C6 C5 Rh1 70.8(6) . y
C4 C5 Rh1 113.2(8) . y
C5 C6 C7 122.5(11) . y
C5 C6 Rh1 68.7(6) . y
C7 C6 Rh1 116.1(7) . y
C6 C7 C8 111.8(8) . y
C1 C8 C7 112.6(8) . y
F4 P1 F6 173.4(10) . y
F4 P1 F5 90.4(8) . y
F6 P1 F5 86.4(8) . y
F4 P1 F1 86.8(7) . y
F6 P1 F1 98.7(9) . y
F5 P1 F1 84.9(7) . y
F4 P1 F3 96.3(9) . y
F6 P1 F3 87.3(7) . y
F5 P1 F3 172.0(9) . y
F1 P1 F3 91.0(6) . y
F4 P1 F2 87.0(7) . y
F6 P1 F2 87.6(8) . y
F5 P1 F2 96.4(8) . y
F1 P1 F2 173.6(8) . y
F3 P1 F2 88.4(6) . y
O41 C41 C43A 116(2) . y
O41 C41 C43B 120.1(19) . y
C43A C41 C43B 73(2) . y
O41 C41 C42 121.1(16) . y
C43A C41 C42 109(2) . y
C43B C41 C42 107.5(15) . 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 C5 2.073(10) . y
Rh1 C6 2.102(10) . y
Rh1 C1 2.114(8) . y
Rh1 N2 2.117(6) . y
Rh1 C2 2.124(9) . y
Rh1 N1 2.158(7) . y
Rh1 N3 2.411(7) . y
N1 C12 1.342(11) . y
N1 C16 1.348(10) . y
N2 C22 1.345(10) . y
N2 C26 1.349(10) . y
N3 C11 1.464(11) . y
N3 C31 1.469(10) . y
N3 C21 1.490(9) . y
C11 C12 1.515(12) . y
C12 C13 1.365(13) . y
C13 C14 1.378(13) . y
C14 C15 1.378(14) . y
C15 C16 1.352(13) . y
C21 C22 1.492(11) . y
C22 C23 1.370(11) . y
C23 C24 1.379(12) . y
C24 C25 1.380(13) . y
C25 C26 1.374(12) . y
C31 C31 1.514(15) 3_655 y
C1 C2 1.378(12) . y
C1 C8 1.498(13) . y
C2 C3 1.531(15) . y
C3 C4 1.480(17) . y
C4 C5 1.492(16) . y
C5 C6 1.446(16) . y
C6 C7 1.488(13) . y
C7 C8 1.511(14) . y
P1 F4 1.486(10) . y
P1 F6 1.489(10) . y
P1 F5 1.498(11) . y
P1 F1 1.503(8) . y
P1 F3 1.516(9) . y
P1 F2 1.548(10) . y
C41 O41 1.154(14) . y
C41 C43A 1.505(18) . y
C41 C43B 1.525(18) . y
C41 C42 1.546(14) . y
