POCOP-Type Pincer Complexes of Nickel: Synthesis, Characterization, and Ligand Exchange Reactivities of New Cationic Acetonitrile Adducts
Lapointe, Sébastien; Vabre, Boris; Zargarian, Davit; Organometallics 34 (2015) 3520–; doi:10.1021/acs.organomet.5b00272

data_4087550
_publ_section_title
;
 POCOP-Type Pincer Complexes of Nickel: Synthesis, Characterization, and
 Ligand Exchange Reactivities of New Cationic Acetonitrile Adducts
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3520
_journal_paper_doi               10.1021/acs.organomet.5b00272
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C21 H36 N Ni O3 P2, C F3 O3 S'
_chemical_formula_sum            'C22 H36 F3 N Ni O6 P2 S'
_chemical_formula_weight         620.23
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.384(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8233(6)
_cell_length_b                   30.142(2)
_cell_length_c                   12.1730(9)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.67
_cell_measurement_theta_min      3.63
_cell_volume                     2869.7(4)
_computing_cell_refinement       'Bruker SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'Bruker SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'Bruker SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            112735
_diffrn_reflns_theta_full        71.08
_diffrn_reflns_theta_max         71.08
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    3.204
_exptl_absorpt_correction_T_max  0.8068
_exptl_absorpt_correction_T_min  0.7400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.085(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11028
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.4162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                10932
_reflns_number_total             11028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00272_si_001.cif
_cod_data_source_block           bors56
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2869.6(4)
_cod_original_sg_symbol_H-M      'P2(1)   '
_cod_database_code               4087550