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_4077299
_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         ' 2(C35 H29 Br Ni O2 P2), C H2 Cl2  '
_chemical_formula_sum            'C71 H60 Br2 Cl2 Ni2 O4 P4'
_chemical_formula_weight         1449.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             1999-09-22
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1999-09-30 - Report done on  2(C35 H29 Br Ni O2 P2), C H2 Cl2
             (sample ew287-1)
             by A. David Rae and Anthony C. Willis
             for Eric Wenger and Martin A. Bennett
2001-01-15 - acw edits cif
2001-01-15 - passes checkcif with minor warnings
             data is weak: see _refine_special_details
             R-merge  on 0kl reflections only
             some shift/error ratios large: see _refine_special_details
;
_cell_angle_alpha                90
_cell_angle_beta                 105.55(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.610(4)
_cell_length_b                   15.700(2)
_cell_length_c                   22.175(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      20.4
_cell_volume                     6241.9(18)
_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  RAELS96
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_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 \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00144
_diffrn_orient_matrix_UB_12      0.03355
_diffrn_orient_matrix_UB_13      -0.03799
_diffrn_orient_matrix_UB_21      -0.05426
_diffrn_orient_matrix_UB_22      0.01332
_diffrn_orient_matrix_UB_23      -0.00769
_diffrn_orient_matrix_UB_31      0.01285
_diffrn_orient_matrix_UB_32      0.05248
_diffrn_orient_matrix_UB_33      0.02624
_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  0.20850
_diffrn_reflns_av_sigmaI/netI    0.250
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5022
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        -1.77
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.408
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.39
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.259
_refine_ls_goodness_of_fit_ref   1.64
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1706
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.255
_refine_ls_R_factor_gt           0.094
_refine_ls_shift/su_max          0.7
_refine_ls_shift/su_mean         0.1
_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         0.149
_refine_ls_wR_factor_ref         0.118
_reflns_number_gt                1635
_reflns_number_total             4813
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            om0101083.cif
_cod_data_source_block           exw36
_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        6242(2)
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_original_formula_sum        'C71 H60 Br2 Cl2 Ni2 O4  P4 '
_cod_database_code               4077299