#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:43:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178664 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077597.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_4077597
loop_
_publ_author_name
'Pelagatti, Paolo'
'Bacchi, Alessia'
'Bobbio, Carla'
'Carcelli, Mauro'
'Costa, Mirco'
'Pelizzi, Corrado'
'Vivorio, Cristiano'
_publ_section_title
;
 Synthesis, Characterization, and Reactivity toward MeI of Carbonyl Rh(I)
 Complexes Containing a PNO Hydrazonic Ligand
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5440
_journal_paper_doi               10.1021/om000562r
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C30.5 H23.5 N2 O2 P Rh'
_chemical_formula_weight         583.95
_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                106.750(5)
_cell_angle_beta                 98.440(5)
_cell_angle_gamma                102.950(5)
_cell_formula_units_Z            2
_cell_length_a                   14.051(5)
_cell_length_b                   10.477(5)
_cell_length_c                   9.667(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1293.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Siemens AED diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3158
_diffrn_reflns_theta_full        22.05
_diffrn_reflns_theta_max         22.05
_diffrn_reflns_theta_min         3.05
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.853
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.603
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1615
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.325
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1670P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2648
_reflns_number_gt                1276
_reflns_number_total             3158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000562r.cif
_cod_data_source_block           Compound_3
_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 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077597
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_calc_flag
_atom_site_refinement_flags
Rh Rh 0.67627(7) 0.28898(17) 0.01781(13) 0.1409(9) Uani 1 d .
P P 0.7626(2) 0.1921(5) 0.1420(3) 0.1224(17) Uani 1 d .
O1 O 0.5870(6) 0.3561(13) -0.1161(11) 0.142(4) Uani 1 d .
N1 N 0.5144(8) 0.124(2) -0.2385(12) 0.129(5) Uani 1 d .
N2 N 0.5814(9) 0.109(2) -0.1265(15) 0.133(7) Uani 1 d .
C1 C 0.4574(6) 0.2837(14) -0.3348(9) 0.144(5) Uani 1 d GU
C2 C 0.4490(7) 0.4181(12) -0.3065(10) 0.172(6) Uani 1 d GU
H2 H 0.4834 0.4868 -0.2168 0.206 Uiso 1 calc R
C3 C 0.3891(8) 0.4498(12) -0.4122(12) 0.179(6) Uani 1 d GU
H3 H 0.3835 0.5397 -0.3933 0.214 Uiso 1 calc R
C4 C 0.3376(7) 0.3472(14) -0.5463(10) 0.175(6) Uani 1 d GU
H4 H 0.2976 0.3684 -0.6170 0.210 Uiso 1 calc R
C5 C 0.3461(8) 0.2128(14) -0.5746(8) 0.193(7) Uani 1 d GU
H5 H 0.3116 0.1441 -0.6643 0.231 Uiso 1 calc R
C6 C 0.4060(8) 0.1811(12) -0.4689(10) 0.176(6) Uani 1 d GU
H6 H 0.4116 0.0912 -0.4878 0.211 Uiso 1 calc R
C7 C 0.5262(12) 0.257(3) -0.217(2) 0.134(8) Uani 1 d .
C8 C 0.5773(12) -0.011(3) -0.1315(19) 0.143(9) Uani 1 d .
H8 H 0.5302 -0.0777 -0.2127 0.171 Uiso 1 calc R
C9 C 0.6311(6) -0.0713(13) -0.0360(9) 0.131(5) Uani 1 d GU
C10 C 0.7088(6) 0.0054(10) 0.0874(10) 0.119(4) Uani 1 d GU
C11 C 0.7534(5) -0.0615(11) 0.1721(7) 0.127(5) Uani 1 d GU
H11 H 0.8054 -0.0102 0.2547 0.153 Uiso 1 calc R
C12 C 0.7203(6) -0.2052(11) 0.1334(9) 0.132(5) Uani 1 d GU
H12 H 0.7502 -0.2500 0.1901 0.158 Uiso 1 calc R
C13 C 0.6427(6) -0.2819(10) 0.0100(10) 0.137(4) Uani 1 d GU
H13 H 0.6206 -0.3780 -0.0159 0.164 Uiso 1 calc R
C14 C 0.5981(5) -0.2150(13) -0.0747(8) 0.143(5) Uani 1 d GU
H14 H 0.5461 -0.2663 -0.1573 0.172 Uiso 1 calc R
C15 C 0.7715(6) 0.2513(11) 0.3403(8) 0.117(4) Uani 1 d GU
C16 C 0.8468(6) 0.3696(11) 0.4303(11) 0.133(5) Uani 1 d GU
H16 H 0.8964 0.4114 0.3904 0.160 Uiso 1 calc R
C17 C 0.8479(8) 0.4255(10) 0.5797(11) 0.153(5) Uani 1 d GU
H17 H 0.8983 0.5046 0.6399 0.183 Uiso 1 calc R
C18 C 0.7738(9) 0.3631(12) 0.6393(8) 0.170(6) Uani 1 d GU
H18 H 0.7745 0.4004 0.7393 0.204 Uiso 1 calc R
C19 C 0.6985(7) 0.2448(13) 0.5493(10) 0.157(6) Uani 1 d GU
H19 H 0.6489 0.2030 0.5892 0.188 Uiso 1 calc R
C20 C 0.6974(6) 0.1889(11) 0.3999(10) 0.141(5) Uani 1 d GU
H20 H 0.6470 0.1097 0.3397 0.169 Uiso 1 calc R
C21 C 0.8910(5) 0.2090(12) 0.1237(10) 0.136(5) Uani 1 d GU
C22 C 0.9187(7) 0.2542(14) 0.0098(10) 0.208(7) Uani 1 d GU
H22 H 0.8723 0.2756 -0.0524 0.249 Uiso 1 calc R
C23 C 1.0157(8) 0.2674(15) -0.0112(11) 0.238(8) Uani 1 d GU
H23 H 1.0342 0.2976 -0.0874 0.286 Uiso 1 calc R
C24 C 1.0851(5) 0.2354(14) 0.0818(13) 0.206(8) Uani 1 d GU
H24 H 1.1500 0.2442 0.0677 0.247 Uiso 1 calc R
C25 C 1.0574(6) 0.1902(12) 0.1957(13) 0.180(6) Uani 1 d GU
H25 H 1.1038 0.1688 0.2579 0.216 Uiso 1 calc R
C26 C 0.9604(6) 0.1770(11) 0.2167(10) 0.140(5) Uani 1 d GU
H26 H 0.9418 0.1468 0.2929 0.168 Uiso 1 calc R
C27 C 0.7589(11) 0.452(3) 0.135(3) 0.202(10) Uani 1 d U
O2 O 0.8152(10) 0.5605(19) 0.208(2) 0.270(10) Uani 1 d U
C28 C 0.9180(14) 0.903(2) 0.488(2) 0.234(10) Uiso 1 d D
H28 H 0.8598 0.8357 0.4801 0.280 Uiso 1 calc R
C29 C 0.9275(15) 1.033(3) 0.560(2) 0.222(9) Uiso 1 d D
C30 C 0.991(2) 0.8645(19) 0.425(2) 0.280(12) Uiso 1 d D
H30 H 0.9851 0.7722 0.3732 0.336 Uiso 1 calc R
C31 C 0.859(4) 1.060(4) 0.624(4) 0.28(3) Uiso 0.50 d PD
H31A H 0.7980 0.9863 0.5767 0.413 Uiso 0.50 calc PR
H31B H 0.8487 1.1457 0.6172 0.413 Uiso 0.50 calc PR
H31C H 0.8777 1.0680 0.7262 0.413 Uiso 0.50 calc PR
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'
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
C27 Rh N2 176.2(6) . .
C27 Rh O1 99.3(6) . .
N2 Rh O1 77.5(6) . .
C27 Rh P 87.5(5) . .
N2 Rh P 95.7(4) . .
O1 Rh P 173.1(4) . .
C15 P C21 104.6(4) . .
C15 P C10 103.4(5) . .
C21 P C10 103.1(5) . .
C15 P Rh 114.9(3) . .
C21 P Rh 116.4(3) . .
C10 P Rh 112.9(3) . .
C7 O1 Rh 111.2(12) . .
C7 N1 N2 109.4(15) . .
C8 N2 N1 116.5(18) . .
C8 N2 Rh 128.9(14) . .
N1 N2 Rh 114.6(13) . .
C2 C1 C6 120.0 . .
C2 C1 C7 117.2(13) . .
C6 C1 C7 122.8(13) . .
C1 C2 C3 120.0 . .
C4 C3 C2 120.0 . .
C3 C4 C5 120.0 . .
C4 C5 C6 120.0 . .
C5 C6 C1 120.0 . .
O1 C7 N1 127.2(15) . .
O1 C7 C1 120(2) . .
N1 C7 C1 113(2) . .
N2 C8 C9 133(2) . .
C10 C9 C14 120.0 . .
C10 C9 C8 124.6(12) . .
C14 C9 C8 115.4(12) . .
C9 C10 C11 120.0 . .
C9 C10 P 123.7(5) . .
C11 C10 P 116.2(5) . .
C12 C11 C10 120.0 . .
C13 C12 C11 120.0 . .
C12 C13 C14 120.0 . .
C13 C14 C9 120.0 . .
C16 C15 C20 120.0 . .
C16 C15 P 119.3(6) . .
C20 C15 P 120.3(5) . .
C15 C16 C17 120.0 . .
C16 C17 C18 120.0 . .
C19 C18 C17 120.0 . .
C18 C19 C20 120.0 . .
C19 C20 C15 120.0 . .
C22 C21 C26 120.0 . .
C22 C21 P 117.3(5) . .
C26 C21 P 122.7(5) . .
C23 C22 C21 120.0 . .
C22 C23 C24 120.0 . .
C25 C24 C23 120.0 . .
C24 C25 C26 120.0 . .
C25 C26 C21 120.0 . .
O2 C27 Rh 178(2) . .
C29 C28 C30 121.2(13) . .
C31 C29 C28 117(3) . .
C31 C29 C30 120(3) . 2_776
C28 C29 C30 122.6(13) . 2_776
C29 C30 C28 116.2(12) 2_776 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh C27 1.77(2) .
Rh N2 2.024(18) .
Rh O1 2.046(8) .
Rh P 2.184(4) .
P C15 1.813(7) .
P C21 1.813(6) .
P C10 1.817(10) .
O1 C7 1.23(2) .
N1 C7 1.32(2) .
N1 N2 1.399(17) .
N2 C8 1.23(2) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C1 C7 1.515(15) .
C2 C3 1.3900 .
C3 C4 1.3900 .
C4 C5 1.3900 .
C5 C6 1.3900 .
C8 C9 1.472(18) .
C9 C10 1.3900 .
C9 C14 1.3900 .
C10 C11 1.3900 .
C11 C12 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C15 C16 1.3900 .
C15 C20 1.3900 .
C16 C17 1.3900 .
C17 C18 1.3900 .
C18 C19 1.3900 .
C19 C20 1.3900 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C23 C24 1.3900 .
C24 C25 1.3900 .
C25 C26 1.3900 .
C27 O2 1.18(2) .
C28 C29 1.307(15) .
C28 C30 1.349(17) .
C29 C31 1.26(4) .
C29 C30 1.338(17) 2_776
C30 C29 1.338(16) 2_776
