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_4077303
_publ_contact_author_name        'Alison Edwards'
_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_compound_source        'Local laboratory'
_chemical_formula_moiety         'C45 H40 Br F3 Ni O2 P2 '
_chemical_formula_sum            'C45 H40 Br F3 Ni O2 P2'
_chemical_formula_weight         870.374
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           'maXus + CRYSTALS_ver_12-03-99'
_audit_update_record
;
Notes:
Poor quality crystal limited diffraction - a highly restrained refinement
has yielded a structure which indicates the chemical composition quite
clearly, phenyl rings geometry has been imposed ie bond length, angle and
planarity.

Checkcif yields the expected alerts regarding resolution and shifts &#x000C
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.506(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.914(2)
_cell_length_b                   15.4458(10)
_cell_length_c                   18.9929(12)
_cell_measurement_reflns_used    184268
_cell_measurement_temperature    200
_cell_measurement_theta_max      23.534
_cell_measurement_theta_min      2.910
_cell_volume                     8076.4(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;

 CAMERON (Watkin, Prout & Pearce,  1996)

;
_computing_publication_material
;

CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)

;
_computing_structure_refinement
;

CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)

;
_computing_structure_solution    'DIRDIF (Buerskens et al., 1992)'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.00372
_diffrn_orient_matrix_UB_12      -0.06221
_diffrn_orient_matrix_UB_13      -0.01446
_diffrn_orient_matrix_UB_21      -0.00899
_diffrn_orient_matrix_UB_22      -0.01464
_diffrn_orient_matrix_UB_23      0.04742
_diffrn_orient_matrix_UB_31      -0.03500
_diffrn_orient_matrix_UB_32      0.01037
_diffrn_orient_matrix_UB_33      -0.01979
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17820
_diffrn_reflns_theta_max         23.47
_exptl_absorpt_coefficient_mu    1.60
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'dark orange - red'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular chunk'
_exptl_crystal_F_000             3567
_refine_diff_density_max         1.46
_refine_diff_density_min         -0.95
_refine_ls_extinction_coef       520.9(1152)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.8975
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     488
_refine_ls_number_reflns         4043
_refine_ls_R_factor_gt           0.1242
_refine_ls_shift/su_max          0.064256
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
 2.69    0.366     1.92
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0985
_reflns_d_resolution_high        0.67
_reflns_d_resolution_low         1.80
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4043
_reflns_number_total             5779
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            om0101083.cif
_cod_data_source_block           exw10z
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1715 2011-07-08 13:25:40Z adriana

Fixed syntax errors related with wrongly placed semicolons miguel 
;
_cod_original_cell_volume        8076.4(8)
_cod_original_sg_symbol_H-M      'C 2/c         '
_cod_original_formula_sum        'C45 H40 Br F3 Ni O2 P2 '
_cod_database_code               4077303