Regioselectivities of the Insertion Reactions of Unsymmetrical Alkynes with the Nickelacycles [NiBr(C6H4CH2PPh2-2)(L)] (L = Tertiary Phosphine)
Edwards, Alison J.; Macgregor, Stuart A.; Rae, A. David; Wenger, Eric; Willis, Anthony C.; Organometallics 20 (2001) 2864–; doi:10.1021/om0101083

data_4077300
_publ_section_title
;
 Regioselectivities of the Insertion Reactions of Unsymmetrical Alkynes
 with the Nickelacycles [NiBr(C6H4CH2PPh2-2)(L)] (L = Tertiary Phosphine)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2864
_journal_paper_doi               10.1021/om0101083
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C44 H41 Br Ni O2 P2, 0.5(C6 H6)'
_chemical_formula_sum            'C47 H44 Br Ni O2 P2'
_chemical_formula_weight         841.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             1999-04-22
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1999-04-16 - Report done on  C47 H44 Br Ni O2 P2
             by Anthony C. Willis
             for Eric Wenger and Martin A. Bennett
2001-01-15 - acw edits cif
2001-01-15 - passes checkcif with minor warnings
;
_cell_angle_alpha                76.36(2)
_cell_angle_beta                 75.75(2)
_cell_angle_gamma                77.03(2)
_cell_formula_units_Z            2
_cell_length_a                   9.776(3)
_cell_length_b                   14.482(4)
_cell_length_c                   15.326(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      55.1
_cell_measurement_theta_min      50.1
_cell_volume                     2011.6(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.08208
_diffrn_orient_matrix_UB_12      -0.03495
_diffrn_orient_matrix_UB_13      -0.04014
_diffrn_orient_matrix_UB_21      0.06830
_diffrn_orient_matrix_UB_22      0.02994
_diffrn_orient_matrix_UB_23      0.01877
_diffrn_orient_matrix_UB_31      0.00977
_diffrn_orient_matrix_UB_32      -0.05562
_diffrn_orient_matrix_UB_33      0.05235
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.05214
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6219
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        1.72
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.903
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             870.00
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.916
_refine_ls_goodness_of_fit_ref   1.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.0200
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0632
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                5330
_reflns_number_total             5960
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            om0101083.cif
_cod_data_source_block           exw40_in_oil_low_T
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2012(1)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C47 H44 Br Ni O2 P2 '
_cod_database_code               4077300