Effects of substituents on the formation of rhenium carbyne and η2-vinyl complexes from the reactions of ReH5(PMe2Ph)3 with terminal alkynes
He, Guomei; Fan, Ting; Chen, Jiangxi; Sung, Herman Ho-Yung; Williams, Ian Duncan; Lin, Zhenyang; Jia, Guochen; New Journal of Chemistry 37 (2013) 1823–; doi:10.1039/c3nj00062a

data_7053127
_publ_section_title
;
 Effects of substituents on the formation of rhenium carbyne and \h2-vinyl
 complexes from the reactions of ReH5(PMe2Ph)3 with terminal alkynes
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1823
_journal_paper_doi               10.1039/c3nj00062a
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C33 H39 Cl2 F3 P3 Re, 0.25(C H3 O H)'
_chemical_formula_sum            'C33.25 H40 Cl2 F3 O0.25 P3 Re'
_chemical_formula_weight         850.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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_date             2012-05-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled May 9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.643(3)
_cell_angle_beta                 98.261(2)
_cell_angle_gamma                108.650(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7952(3)
_cell_length_b                   12.6871(4)
_cell_length_c                   13.8264(4)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.4416
_cell_measurement_theta_min      4.7141
_cell_volume                     1772.30(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
1 omega 38.00 65.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 -120.0000 27
2 omega -24.00 40.00 1.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 0.0000 64
3 omega -75.00 14.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 57.0000 -30.0000 89
4 omega 46.00 120.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 57.0000 60.0000 74
5 omega 4.00 71.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 -38.0000 60.0000 67
6 omega -141.00 -65.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 178.0000 -60.0000 76
7 omega -131.00 -34.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 -77.0000 -150.0000 97
8 omega 40.00 65.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -30.0000 25
9 omega 123.00 149.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -93.0000 26.0000 26
10 omega 41.00 68.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 -150.0000 27
11 omega 40.00 66.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 30.0000 26
12 omega 40.00 67.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -60.0000 27
13 omega 38.00 71.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 60.0000 33
14 omega 38.00 69.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 -180.0000 31
15 omega 37.00 63.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 90.0000 26
16 omega 44.00 69.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 0.0000 25
17 omega 45.00 82.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 -90.0000 37
18 omega 42.00 71.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -38.0000 120.0000 29
19 omega 47.00 176.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 0.0000 -60.0000 129
20 omega 40.00 102.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -93.0000 26.0000 62
21 omega 95.00 177.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 64.0000 -30.0000 82
22 omega 50.00 148.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -92.0000 90.0000 98
23 omega 53.00 130.00 1.0000 17.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -93.0000 -112.0000 77
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0184868000
_diffrn_orient_matrix_UB_12      0.1133234000
_diffrn_orient_matrix_UB_13      -0.0453797000
_diffrn_orient_matrix_UB_21      -0.0403129000
_diffrn_orient_matrix_UB_22      -0.0589572000
_diffrn_orient_matrix_UB_23      -0.1031739000
_diffrn_orient_matrix_UB_31      -0.1458773000
_diffrn_orient_matrix_UB_32      -0.0129310000
_diffrn_orient_matrix_UB_33      0.0044350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10283
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.98
_diffrn_reflns_theta_min         5.46
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    9.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             845
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                6070
_reflns_number_total             6168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00062a.txt
_cod_data_source_block           chen134cult_cpd10
_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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1772.30(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053127
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13