Activation of heteroallenes by coordinatively unsaturated nickel(ii) alkyl complexes supported by the hydrotris(3-phenyl-5-methyl)pyrazolyl borate (Tp(Ph,Me)) ligand.
Abubekerov, Mark; Eymann, Léonard Y M; Gianetti, Thomas L.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14581–14590; doi:10.1039/c6dt01585a

data_7039646
_publ_section_title
;
 Activation of heteroallenes by coordinatively unsaturated nickel(ii)
 alkyl complexes supported by the hydrotris(3-phenyl-5-methyl)pyrazolyl
 borate (Tp(Ph,Me)) ligand.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14581
_journal_page_last               14590
_journal_paper_doi               10.1039/c6dt01585a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H44 B N7 Ni, C4 H10 O'
_chemical_formula_sum            'C46 H54 B N7 Ni O'
_chemical_formula_weight         790.48
_chemical_melting_point          449.0(7)
_chemical_name_common            'Complex 5a'
_chemical_name_systematic        'Complex 5a'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-05-13 deposited with the CCDC.
2016-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.729(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2356(14)
_cell_length_b                   10.7693(10)
_cell_length_c                   24.309(2)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      2.41
_cell_volume                     4248.4(6)
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65820
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_correction_T_min  0.8769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+3.6588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                6886
_reflns_number_total             7831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01585a1.cif
_cod_data_source_block           Complex_5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '448.4 - 449.7' was changed to
'449.0(7)' - the average value was taken and precision was estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039640--7039649.cif.
;
_cod_original_cell_volume        4248.5(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7039646
_solvent_exptl_crystal_recrystallization_method Hexanes