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_4077301
_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         'C39 H31 Br Ni P2 '
_chemical_formula_sum            'C39 H31 Br Ni P2'
_chemical_formula_weight         700.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2000-02-25
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1999 - structure done by Eric Wenger and Lee Welling
2000-02-25 - report and cif done by Tony Willis
2001-01-15 - acw edits cif further
2001-01-15 - passes checkcif with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 96.32(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.870(3)
_cell_length_b                   22.707(4)
_cell_length_c                   13.162(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      36.6
_cell_measurement_theta_min      31.0
_cell_volume                     3229.0(13)
_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      296.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \q 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06988
_diffrn_orient_matrix_UB_12      0.02880
_diffrn_orient_matrix_UB_13      0.01002
_diffrn_orient_matrix_UB_21      -0.05034
_diffrn_orient_matrix_UB_22      0.02568
_diffrn_orient_matrix_UB_23      0.04127
_diffrn_orient_matrix_UB_31      0.03391
_diffrn_orient_matrix_UB_32      -0.02122
_diffrn_orient_matrix_UB_33      0.06356
_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  0.12111
_diffrn_reflns_av_sigmaI/netI    0.130
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5193
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        -1.59
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.467
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1432.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.371
_refine_ls_goodness_of_fit_ref   1.613
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     388
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.0300
_refine_ls_shift/su_mean         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0653
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                2527
_reflns_number_total             4801
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            om0101083.cif
_cod_data_source_block           exw41b
_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        3229(1)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C39 H31 Br Ni P2 '
_cod_database_code               4077301