#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:25:51 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178623 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/34/4073475.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_4073475
loop_
_publ_author_name
'Grotjahn, Douglas B.'
'Zeng, Xi'
'Cooksy, Andrew L.'
'Kassel, W. Scott'
'DiPasquale, Antonio G.'
'Zakharov, Lev. N.'
'Rheingold, Arnold L.'
_publ_section_title
;
 Experimental and Computational Study of the Transformation of Terminal
 Alkynes to Vinylidene Ligands ontrans-(Chloro)bis(phosphine)Rh Fragments
 and Effects of Phosphine Substituents
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3385
_journal_paper_doi               10.1021/om700355r
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C29 H54 Cl N4 O P2 Rh'
_chemical_formula_weight         675.06
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.7930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9000(4)
_cell_length_b                   24.4193(12)
_cell_length_c                   8.9974(4)
_cell_measurement_reflns_used    7611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.43
_cell_volume                     1723.53(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10730
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.9340
_exptl_absorpt_correction_T_min  0.8192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.294
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0270P)²+2.7000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                3683
_reflns_number_total             3928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700355r-file003.cif
_cod_data_source_block           grot88
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4073475
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.0000 0.0000 0.0000 0.02111(9) Uani 1 2 d S
P1 P 0.10066(7) 0.06816(2) 0.16883(6) 0.01749(13) Uani 1 1 d .
Cl1 Cl -0.0887(5) 0.06994(13) -0.1831(3) 0.0361(6) Uani 0.50 1 d P
O1 O -0.0895(16) 0.0816(4) -0.2249(9) 0.039(2) Uani 0.50 1 d P
N1 N 0.3042(3) 0.13119(8) -0.0102(2) 0.0221(4) Uani 1 1 d .
N2 N 0.1954(2) 0.17664(7) 0.1697(2) 0.0181(4) Uani 1 1 d .
C1 C -0.0547(8) 0.0499(3) -0.1343(7) 0.0246(13) Uani 0.50 1 d P
C2 C 0.2005(3) 0.12880(9) 0.1007(2) 0.0184(4) Uani 1 1 d .
C3 C 0.3656(3) 0.18393(10) -0.0104(3) 0.0246(5) Uani 1 1 d .
H3A H 0.4405 0.1985 -0.0756 0.030 Uiso 1 1 calc R
C4 C 0.2983(3) 0.21129(9) 0.1007(2) 0.0196(4) Uani 1 1 d .
C5 C 0.3294(3) 0.26941(9) 0.1544(3) 0.0224(5) Uani 1 1 d .
C6 C 0.4474(7) 0.29803(15) 0.0608(5) 0.0897(19) Uani 1 1 d .
H6A H 0.5555 0.2780 0.0667 0.135 Uiso 1 1 calc R
H6B H 0.4686 0.3354 0.0982 0.135 Uiso 1 1 calc R
H6C H 0.3952 0.2993 -0.0435 0.135 Uiso 1 1 calc R
C7 C 0.1620(5) 0.30005(14) 0.1468(5) 0.0660(13) Uani 1 1 d .
H7A H 0.1165 0.3058 0.0418 0.099 Uiso 1 1 calc R
H7B H 0.1807 0.3356 0.1968 0.099 Uiso 1 1 calc R
H7C H 0.0805 0.2786 0.1968 0.099 Uiso 1 1 calc R
C8 C 0.4071(6) 0.26847(13) 0.3168(4) 0.0659(13) Uani 1 1 d .
H8A H 0.5163 0.2490 0.3251 0.099 Uiso 1 1 calc R
H8B H 0.3295 0.2497 0.3772 0.099 Uiso 1 1 calc R
H8C H 0.4258 0.3061 0.3529 0.099 Uiso 1 1 calc R
C9 C -0.2091(3) 0.12304(12) 0.1550(3) 0.0345(6) Uani 1 1 d .
H9A H -0.2948 0.1405 0.2096 0.052 Uiso 1 1 calc R
H9B H -0.2622 0.0933 0.0928 0.052 Uiso 1 1 calc R
H9C H -0.1619 0.1502 0.0911 0.052 Uiso 1 1 calc R
C10 C -0.0665(3) 0.09989(9) 0.2660(3) 0.0230(5) Uani 1 1 d .
H10A H -0.0139 0.1310 0.3274 0.028 Uiso 1 1 calc R
C11 C -0.1348(3) 0.05873(11) 0.3725(3) 0.0292(5) Uani 1 1 d .
H11A H -0.2275 0.0756 0.4198 0.044 Uiso 1 1 calc R
H11B H -0.0428 0.0480 0.4498 0.044 Uiso 1 1 calc R
H11C H -0.1777 0.0263 0.3161 0.044 Uiso 1 1 calc R
C12 C 0.3155(4) 0.08910(11) 0.4397(3) 0.0309(6) Uani 1 1 d .
H12A H 0.4051 0.0745 0.5138 0.046 Uiso 1 1 calc R
H12B H 0.2163 0.0993 0.4896 0.046 Uiso 1 1 calc R
H12C H 0.3584 0.1215 0.3917 0.046 Uiso 1 1 calc R
C13 C 0.2636(3) 0.04546(9) 0.3213(3) 0.0209(5) Uani 1 1 d .
H13A H 0.2140 0.0141 0.3730 0.025 Uiso 1 1 calc R
C14 C 0.4188(3) 0.02377(12) 0.2535(3) 0.0313(6) Uani 1 1 d .
H14A H 0.5011 0.0087 0.3330 0.047 Uiso 1 1 calc R
H14B H 0.4720 0.0537 0.2034 0.047 Uiso 1 1 calc R
H14C H 0.3829 -0.0050 0.1806 0.047 Uiso 1 1 calc R
C15 C 0.3474(4) 0.08850(11) -0.1129(3) 0.0326(6) Uani 1 1 d .
H15A H 0.3179 0.0526 -0.0746 0.049 Uiso 1 1 calc R
H15B H 0.4699 0.0898 -0.1213 0.049 Uiso 1 1 calc R
H15C H 0.2834 0.0945 -0.2117 0.049 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'
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
C1 Rh1 C1 179.999(1) . 3
C1 Rh1 P1 89.41(19) . .
C1 Rh1 P1 90.60(19) 3 .
C1 Rh1 P1 90.59(19) . 3
C1 Rh1 P1 89.40(19) 3 3
P1 Rh1 P1 179.999(19) . 3
C1 Rh1 Cl1 177.4(2) . 3
C1 Rh1 Cl1 2.6(2) 3 3
P1 Rh1 Cl1 90.64(8) . 3
P1 Rh1 Cl1 89.36(8) 3 3
C1 Rh1 Cl1 2.6(2) . .
C1 Rh1 Cl1 177.4(2) 3 .
P1 Rh1 Cl1 89.35(8) . .
P1 Rh1 Cl1 90.65(8) 3 .
Cl1 Rh1 Cl1 180.0 3 .
C2 P1 C10 100.48(10) . .
C2 P1 C13 101.66(10) . .
C10 P1 C13 104.43(11) . .
C2 P1 Rh1 119.38(7) . .
C10 P1 Rh1 113.71(8) . .
C13 P1 Rh1 115.02(8) . .
C1 Cl1 Rh1 6.6(6) . .
C2 N1 C3 106.43(19) . .
C2 N1 C15 129.6(2) . .
C3 N1 C15 124.0(2) . .
C2 N2 C4 106.21(18) . .
Cl1 C1 O1 10.2(9) . .
Cl1 C1 Rh1 170.8(8) . .
O1 C1 Rh1 178.2(9) . .
N2 C2 N1 111.03(19) . .
N2 C2 P1 121.42(16) . .
N1 C2 P1 127.09(17) . .
C4 C3 N1 106.9(2) . .
C3 C4 N2 109.5(2) . .
C3 C4 C5 129.3(2) . .
N2 C4 C5 121.2(2) . .
C6 C5 C4 110.3(2) . .
C6 C5 C7 110.0(3) . .
C4 C5 C7 110.0(2) . .
C6 C5 C8 109.9(3) . .
C4 C5 C8 109.0(2) . .
C7 C5 C8 107.6(3) . .
C9 C10 C11 111.5(2) . .
C9 C10 P1 111.17(18) . .
C11 C10 P1 110.30(16) . .
C14 C13 C12 111.0(2) . .
C14 C13 P1 109.18(17) . .
C12 C13 P1 114.42(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C1 1.735(7) .
Rh1 C1 1.735(7) 3
Rh1 P1 2.3291(6) .
Rh1 P1 2.3291(6) 3
Rh1 Cl1 2.419(3) 3
Rh1 Cl1 2.419(3) .
P1 C2 1.818(2) .
P1 C10 1.839(2) .
P1 C13 1.851(2) .
Cl1 C1 0.690(6) .
O1 C1 1.133(8) .
N1 C2 1.365(3) .
N1 C3 1.376(3) .
N1 C15 1.460(3) .
N2 C2 1.326(3) .
N2 C4 1.372(3) .
C3 C4 1.362(3) .
C4 C5 1.510(3) .
C5 C6 1.501(4) .
C5 C7 1.513(4) .
C5 C8 1.517(4) .
C9 C10 1.523(4) .
C10 C11 1.530(3) .
C12 C13 1.529(3) .
C13 C14 1.527(3) .
