Reductive Carbonylation of Oxorhenium Hydrides Induced by Lewis Acids
Lambic, Nikola S.; Lilly, Cassandra P.; Robbins, Leanna K.; Sommer, Roger D.; Ison, Elon A.; Organometallics 35 (2016) 2822–; doi:10.1021/acs.organomet.6b00393

data_4088763
_publ_section_title
;
 Reductive Carbonylation of Oxorhenium Hydrides Induced by Lewis Acids
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2822
_journal_paper_doi               10.1021/acs.organomet.6b00393
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C34 H41 N3 O3 Re, B F4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C34.5 H42 B Cl F4 N3 O3 Re'
_chemical_formula_weight         855.17
_chemical_name_common            DippBF3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                80.728(2)
_cell_angle_beta                 77.828(2)
_cell_angle_gamma                83.623(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1424(3)
_cell_length_b                   9.8897(4)
_cell_length_c                   20.4731(7)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.8518
_cell_measurement_theta_min      2.1974
_cell_volume                     1780.12(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6247
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.547
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS V2012/1 (Bruker AXS Inc.)'
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
 ------------------------------------------------------------------

 Equivalent reflections defined according to point group -1    

 Reading batch  1 from file rds495_0m.mul

  2 twin components present

 Mean and maximum errors in direction cosine check function =   0.001   0.007
 The mean error should not exceed 0.008, and is usually caused by matrix
 changes during data processing.

 Maximum 2-theta =  57.69 deg.   Approximate wavelength = 0.71121 Angstroms
 Approximate highest resolution = 0.737 Angstroms
 Approximate unit-cell:   9.173   9.931  20.563   80.68   77.84   83.42

 ==============================================================================

 PART 1 - Refinement of parameters to model systematic errors

     3193 data (   1015 unique ) involve domain  1 only,  mean I/sigma  24.5
     3194 data (   1012 unique ) involve domain  2 only,  mean I/sigma   8.1
    35884 data (   8675 unique ) involve   2 domains,  mean I/sigma  12.0
       20 data (     20 unique ) involve   3 domains,  mean I/sigma   8.3

 Settings for parameter refinement:

 Maximum resolution =  0.1000 A
 (Intensity/sigma) threshold = 1.500
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   3   6

 Refinement of a single parameter set to fit all single and composite
 reflections that contain at least one contribution from domain 1
 ---------------------------------------------------------------------------

    2724 single and  32396 composite reflections used for parameter fitting
 Effective data to parameter ratio =    9.44

 wR2(int) =  0.0677 (selected reflections only, before parameter refinement)

 Cycle wR2(incid) wR2(diffr) Mean wt.
    1    0.0673    0.0584    0.9359
    2    0.0562    0.0550    0.9434
...
   40    0.0540    0.0540    0.9442

 wR2(int) =  0.0540 (selected reflections only, after parameter refinement)

 ==============================================================================

 PART 2 - Reject outliers and establish error model

 Rejected reflections are ignored in the statistics and Postscript plots
 (except the detector diagnostics) and in the output .hkl files. All statistics
 and error estimates refer to total intensities (of single or composite
 reflections) only. Before applying rejections there are:

   42291 total and  10722 unique reflections assuming Friedel's law.

   42290 total and  10722 unique reflections after rejecting pathological cases 

   42262 total and  10722 unique reflections left after |I-<I>|/su test

 g = 0.0416 gave best error model; g set to 0.0416 for further calculations

 ==============================================================================

 PART 3 - Output Postscript diagnostics and corrected data

 Diagnostic plots written to Postscript file twin.eps

 The R(int) and R(sigma) plots are based on all singles and composites,
 <|E^2-1|> is calculated for all individual contributions from domain 1
 assuming SAINT partitioning and the chi^2 and spatial plots show only
 those single and composite reflections actually fitted.

 Unique HKLF 4 data extracted from all observations involving domain 1

 Cycle   N(1) Rint(1)  N(all) Rint(all) Twin fractions
    1   38445  0.1696   41616  0.1677   0.8721  0.1279
    2   38445  0.0447   41616  0.0457   0.8590  0.1410
    ...
   19   38445  0.0387   41616  0.0395   0.8537  0.1463
   20   38445  0.0387   41616  0.0395   0.8537  0.1463

 N(1) and Rint(1) refer to singles and composites that include domain 1.

 Rint = 0.0395  for all   41616  observations and
 Rint = 0.0327  for all   21913  observations with I > 3sigma(I)

 Rint is based on agreement between observed single and composite intensities
 and those calculated from refined unique intensities and twin fractions.

    8634 Corrected reflections written to file twin4.hkl
 Reflections merged according to point-group -1    
 Minimum and maximum apparent transmission:  0.580772  0.745760
 Additional spherical absorption correction applied with mu*r =  0.2000

 HKLF 5 dataset constructed from all observations involving domain 1
   17550 Corrected reflections written to file twin5.hkl
 Reflections merged according to point-group -1    
 Single reflections that also occur in composites omitted
 Minimum and maximum apparent transmission:  0.579504  0.745760
 Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.599
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+1.9740P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                6122
_reflns_number_total             6247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00393_si_002.cif
_cod_data_source_block           rds495
_cod_original_formula_sum        'C34.50 H42 B Cl F4 N3 O3 Re'
_cod_database_code               4088763
_shelx_res_checksum              17612
_shelx_hkl_checksum              32231