#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:29:10 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195007 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/52/1545281.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_1545281
loop_
_publ_author_name
'Pell, Christopher J.'
'Zhu, Yanjun'
'Huacuja, Rafael'
'Herbert, David E.'
'Hughes, Russell P.'
'Ozerov, Oleg V.'
_publ_section_title
;
 Fluorocarbene, fluoroolefin, and fluorocarbyne complexes of Rh
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              3178
_journal_paper_doi               10.1039/C6SC05391B
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         none
_chemical_formula_sum            'C27 H40 F2 N P2 Rh'
_chemical_formula_weight         581.45
_chemical_melting_point          ?
_chemical_name_common            none(PNP)Rh=CF2
_chemical_name_systematic        (PNP)Rh=CF2
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.693(6)
_cell_length_b                   16.565(6)
_cell_length_c                   9.888(4)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.40
_cell_volume                     2734.2(18)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30909
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.8932
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: isooctane'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0357
_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)+(0.0335P)²+0.3326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                5169
_reflns_number_total             6606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc05391b2.cif
_cod_data_source_block           oz342
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1545280--1545282.cif.
;
_cod_original_cell_volume        2734.1(18)
_cod_original_sg_symbol_H-M      p_n_a_21
_cod_database_code               1545281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'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
Rh1 Rh 0.251682(16) 0.959609(14) 0.16249(5) 0.01973(7) Uani 1 1 d .
P1 P 0.32060(6) 0.98615(6) 0.35934(10) 0.0227(2) Uani 1 1 d .
F1 F 0.29340(17) 1.03835(16) -0.0855(2) 0.0487(7) Uani 1 1 d .
N1 N 0.20589(17) 0.86926(18) 0.2801(3) 0.0202(6) Uani 1 1 d .
C1 C 0.3032(2) 1.0288(2) 0.0489(4) 0.0287(9) Uani 1 1 d .
P2 P 0.15420(5) 0.91813(6) 0.01332(9) 0.02001(19) Uani 1 1 d .
F2 F 0.36703(16) 1.07566(18) 0.0706(3) 0.0560(8) Uani 1 1 d .
C2 C 0.3114(2) 0.8891(2) 0.4433(4) 0.0221(8) Uani 1 1 d .
C3 C 0.3601(2) 0.8605(2) 0.5454(4) 0.0244(8) Uani 1 1 d .
H3A H 0.3989 0.8960 0.5830 0.029 Uiso 1 1 calc R
C4 C 0.3551(2) 0.7821(2) 0.5959(4) 0.0269(9) Uani 1 1 d .
C5 C 0.2977(2) 0.7325(2) 0.5368(4) 0.0247(8) Uani 1 1 d .
H5A H 0.2932 0.6782 0.5668 0.030 Uiso 1 1 calc R
C6 C 0.2471(2) 0.7594(2) 0.4361(4) 0.0214(9) Uani 1 1 d .
H6A H 0.2084 0.7236 0.3992 0.026 Uiso 1 1 calc R
C7 C 0.25178(19) 0.8386(2) 0.3871(3) 0.0197(7) Uani 1 1 d .
C8 C 0.4116(2) 0.7521(3) 0.7025(4) 0.0347(10) Uani 1 1 d .
H8A H 0.4476 0.7960 0.7299 0.052 Uiso 1 1 calc R
H8B H 0.4433 0.7072 0.6662 0.052 Uiso 1 1 calc R
H8C H 0.3810 0.7335 0.7811 0.052 Uiso 1 1 calc R
C9 C 0.1306(2) 0.8356(2) 0.2489(3) 0.0188(7) Uani 1 1 d .
C10 C 0.0816(2) 0.7956(2) 0.3446(4) 0.0232(8) Uani 1 1 d .
H10A H 0.0999 0.7887 0.4348 0.028 Uiso 1 1 calc R
C11 C 0.0073(2) 0.7666(2) 0.3077(4) 0.0257(9) Uani 1 1 d .
H11A H -0.0242 0.7396 0.3737 0.031 Uiso 1 1 calc R
C12 C -0.0233(2) 0.7752(2) 0.1781(4) 0.0256(8) Uani 1 1 d .
C13 C 0.0229(2) 0.8181(2) 0.0863(4) 0.0254(8) Uani 1 1 d .
H13A H 0.0032 0.8259 -0.0028 0.031 Uiso 1 1 calc R
C14 C 0.0976(2) 0.8501(2) 0.1211(3) 0.0201(8) Uani 1 1 d .
C15 C -0.1041(2) 0.7433(2) 0.1396(4) 0.0360(10) Uani 1 1 d .
H15A H -0.1275 0.7146 0.2168 0.054 Uiso 1 1 calc R
H15B H -0.0985 0.7061 0.0631 0.054 Uiso 1 1 calc R
H15C H -0.1390 0.7883 0.1139 0.054 Uiso 1 1 calc R
C16 C 0.1853(2) 0.8612(2) -0.1367(4) 0.0255(8) Uani 1 1 d .
H16A H 0.2200 0.8978 -0.1918 0.031 Uiso 1 1 calc R
C17 C 0.2372(3) 0.7919(4) -0.0906(5) 0.0422(12) Uani 1 1 d .
H17A H 0.2552 0.7610 -0.1695 0.063 Uiso 1 1 calc R
H17B H 0.2064 0.7568 -0.0304 0.063 Uiso 1 1 calc R
H17C H 0.2840 0.8131 -0.0421 0.063 Uiso 1 1 calc R
C18 C 0.1191(2) 0.8312(3) -0.2289(4) 0.0347(10) Uani 1 1 d .
H18A H 0.1426 0.8026 -0.3059 0.052 Uiso 1 1 calc R
H18B H 0.0878 0.8773 -0.2617 0.052 Uiso 1 1 calc R
H18C H 0.0840 0.7945 -0.1786 0.052 Uiso 1 1 calc R
C19 C 0.0772(2) 0.9896(2) -0.0465(4) 0.0235(8) Uani 1 1 d .
H19A H 0.0324 0.9573 -0.0864 0.028 Uiso 1 1 calc R
C20 C 0.1086(2) 1.0456(2) -0.1558(4) 0.0294(9) Uani 1 1 d .
H20A H 0.0657 1.0821 -0.1849 0.044 Uiso 1 1 calc R
H20B H 0.1269 1.0136 -0.2332 0.044 Uiso 1 1 calc R
H20C H 0.1534 1.0773 -0.1200 0.044 Uiso 1 1 calc R
C21 C 0.0433(3) 1.0373(2) 0.0721(4) 0.0367(10) Uani 1 1 d .
H21A H 0.0022 1.0748 0.0392 0.055 Uiso 1 1 calc R
H21B H 0.0864 1.0678 0.1158 0.055 Uiso 1 1 calc R
H21C H 0.0193 1.0000 0.1375 0.055 Uiso 1 1 calc R
C22 C 0.2644(3) 1.0586(3) 0.4658(4) 0.0311(10) Uani 1 1 d .
H22A H 0.2704 1.1130 0.4231 0.037 Uiso 1 1 calc R
C23 C 0.1747(3) 1.0382(3) 0.4639(4) 0.0377(11) Uani 1 1 d .
H23A H 0.1455 1.0772 0.5197 0.057 Uiso 1 1 calc R
H23B H 0.1666 0.9837 0.5001 0.057 Uiso 1 1 calc R
H23C H 0.1548 1.0406 0.3708 0.057 Uiso 1 1 calc R
C24 C 0.2957(3) 1.0655(3) 0.6098(4) 0.0396(11) Uani 1 1 d .
H24A H 0.2634 1.1050 0.6597 0.059 Uiso 1 1 calc R
H24B H 0.3516 1.0833 0.6080 0.059 Uiso 1 1 calc R
H24C H 0.2921 1.0128 0.6544 0.059 Uiso 1 1 calc R
C25 C 0.4266(2) 1.0137(2) 0.3817(4) 0.0319(10) Uani 1 1 d .
H25A H 0.4413 1.0001 0.4771 0.038 Uiso 1 1 calc R
C26 C 0.4428(3) 1.1038(3) 0.3626(5) 0.0503(13) Uani 1 1 d .
H26A H 0.5000 1.1146 0.3765 0.075 Uiso 1 1 calc R
H26B H 0.4114 1.1347 0.4283 0.075 Uiso 1 1 calc R
H26C H 0.4276 1.1198 0.2708 0.075 Uiso 1 1 calc R
C27 C 0.4794(2) 0.9626(3) 0.2899(5) 0.0427(12) Uani 1 1 d .
H27A H 0.5356 0.9776 0.3034 0.064 Uiso 1 1 calc R
H27B H 0.4644 0.9720 0.1954 0.064 Uiso 1 1 calc R
H27C H 0.4721 0.9054 0.3119 0.064 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'
F F 0.0171 0.0103 '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'
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
C1 Rh1 N1 171.39(15)
C1 Rh1 P2 97.29(13)
N1 Rh1 P2 83.19(9)
C1 Rh1 P1 99.49(13)
N1 Rh1 P1 81.13(9)
P2 Rh1 P1 162.14(4)
C2 P1 C25 104.26(18)
C2 P1 C22 105.72(19)
C25 P1 C22 104.95(19)
C2 P1 Rh1 100.07(12)
C25 P1 Rh1 128.99(14)
C22 P1 Rh1 110.54(14)
C7 N1 C9 120.6(3)
C7 N1 Rh1 119.4(2)
C9 N1 Rh1 119.9(2)
F2 C1 F1 100.8(3)
F2 C1 Rh1 130.1(3)
F1 C1 Rh1 128.6(3)
C14 P2 C16 107.62(17)
C14 P2 C19 102.95(17)
C16 P2 C19 105.58(17)
C14 P2 Rh1 100.20(12)
C16 P2 Rh1 118.15(13)
C19 P2 Rh1 120.42(13)
C3 C2 C7 120.0(3)
C3 C2 P1 126.0(3)
C7 C2 P1 113.8(3)
C2 C3 C4 123.1(3)
C5 C4 C3 116.2(3)
C5 C4 C8 122.2(4)
C3 C4 C8 121.6(4)
C6 C5 C4 122.3(3)
C5 C6 C7 121.2(3)
N1 C7 C6 124.8(3)
N1 C7 C2 117.8(3)
C6 C7 C2 117.2(3)
C14 C9 N1 118.8(3)
C14 C9 C10 117.1(3)
N1 C9 C10 123.7(3)
C11 C10 C9 120.4(4)
C10 C11 C12 122.7(4)
C13 C12 C11 116.9(3)
C13 C12 C15 121.1(4)
C11 C12 C15 122.0(4)
C12 C13 C14 122.0(3)
C13 C14 C9 120.6(3)
C13 C14 P2 123.7(3)
C9 C14 P2 115.5(3)
C17 C16 C18 110.6(3)
C17 C16 P2 108.1(3)
C18 C16 P2 116.6(3)
C20 C19 C21 111.1(3)
C20 C19 P2 112.3(3)
C21 C19 P2 110.2(3)
C24 C22 C23 111.3(4)
C24 C22 P1 114.0(3)
C23 C22 P1 110.2(3)
C27 C25 C26 111.5(4)
C27 C25 P1 110.3(3)
C26 C25 P1 113.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 C1 1.821(4)
Rh1 N1 2.043(3)
Rh1 P2 2.3012(11)
Rh1 P1 2.3033(12)
P1 C2 1.816(4)
P1 C25 1.840(4)
P1 C22 1.852(4)
F1 C1 1.348(5)
N1 C7 1.402(4)
N1 C9 1.409(4)
C1 F2 1.335(4)
P2 C14 1.816(4)
P2 C16 1.833(4)
P2 C19 1.845(4)
C2 C3 1.380(5)
C2 C7 1.413(5)
C3 C4 1.393(5)
C4 C5 1.392(5)
C4 C8 1.500(5)
C5 C6 1.379(5)
C6 C7 1.400(5)
C9 C14 1.399(5)
C9 C10 1.417(5)
C10 C11 1.379(5)
C11 C12 1.388(6)
C12 C13 1.386(5)
C12 C15 1.497(5)
C13 C14 1.399(5)
C16 C17 1.508(6)
C16 C18 1.517(5)
C19 C20 1.518(5)
C19 C21 1.523(5)
C22 C24 1.521(6)
C22 C23 1.535(6)
C25 C27 1.522(6)
C25 C26 1.528(5)
