Evaluating the Effect of Catalyst Nuclearity in Ni-Catalyzed Alkyne Cyclotrimerizations.
Pal, Sudipta; Uyeda, Christopher; Journal of the American Chemical Society 137 (2015) 8042–8045; doi:10.1021/jacs.5b04990

data_4123927
_publ_section_title
;
 Evaluating the Effect of Catalyst Nuclearity in Ni-Catalyzed Alkyne
 Cyclotrimerizations.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8042
_journal_page_last               8045
_journal_paper_doi               10.1021/jacs.5b04990
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         C41,H54,N4,Ni2,Si1
_chemical_formula_sum            'C41 H54 N4 Ni2 Si'
_chemical_formula_weight         748.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                107.132(4)
_cell_angle_beta                 93.402(3)
_cell_angle_gamma                102.319(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2242(3)
_cell_length_b                   14.3806(7)
_cell_length_c                   17.7803(6)
_cell_measurement_reflns_used    46579
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.910
_cell_measurement_theta_min      4.835
_cell_volume                     1946.39(15)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla, et. al., 2005)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46579
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.910
_diffrn_reflns_theta_min         4.835
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       cube
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0794P)^2^+1.2763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6369
_reflns_number_total             6835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04990_si_001.cif
_cod_data_source_block           complex7
_cod_original_cell_volume        1946.39(14)
_cod_database_code               4123927
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              3619
_shelx_hkl_checksum              33575