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_4087549
_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
'0.67(C21 H36 N Ni O2 P2), 0.17(C43.35 H72 F4.04 N2 Ni2 O8.04 P4 S1.35), 0.78(C F3 O3 S)'
_chemical_formula_sum            'C22 H36 F3 N Ni O5 P2 S'
_chemical_formula_weight         604.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.2664(5)
_cell_length_b                   29.5903(8)
_cell_length_c                   18.8491(5)
_cell_measurement_reflns_used    9045
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.75
_cell_measurement_theta_min      2.83
_cell_volume                     8694.3(4)
_computing_cell_refinement
'SAINT (2009) V7.68A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
;
APEX 2 (2009) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
'SAINT (2009) V7.68A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker Platinum 135 CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Microstar X8'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            170890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.068
_diffrn_reflns_theta_min         2.835
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Bruker Microstar/FR591 generator'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.130
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0698 after correction.
The Ratio of minimum to maximum transmission is 0.8427.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.499
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         16417
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+13.1090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14732
_reflns_number_total             16417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00272_si_001.cif
_cod_data_source_block           selap1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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_database_code               4087549
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C66A) = Uanis(C66B)
Uanis(C65A) = Uanis(C65B)
Uanis(F6A) = Uanis(F6B)
Uanis(F7A) = Uanis(F7B)
Uanis(F8A) = Uanis(F8B)
Uanis(F9A) = Uanis(F9B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5A) = Uanis(F5B)
Uanis(N3A) = Uanis(N3B)
3. Others
 Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37B)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Sof(C38B)=Sof(H38B)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40B)=
 Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40A)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(S3B)=Sof(O13B)=Sof(O14B)=Sof(O15B)=Sof(C66B)=Sof(F8B)=Sof(F7B)=Sof(F9B)=1-
 FVAR(3)
 Sof(C66A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(O14A)=Sof(O13A)=Sof(O15A)=Sof(S3A)=
 FVAR(3)
 Sof(S2B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(C65B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-
 FVAR(4)
 Sof(S2A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C65A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 FVAR(4)
 Sof(C50B)=Sof(H50B)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52B)=
 Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(5)
 Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52A)=
 Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(5)
 Sof(N3B)=Sof(C62B)=Sof(C63B)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(6)
 Sof(N3A)=Sof(C62A)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(6)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C32(H32), C29(H29), C56(H56), C53(H53),
 C59(H59), C50A(H50A), C50B(H50B), C35A(H35A), C35B(H35B), C38A(H38A),
 C38B(H38B)
4.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C), C54(H54A,H54B,H54C),
 C60(H60A,H60B,H60C), C55(H55A,H55B,H55C), C15(H15A,H15B,H15C), C36A(H36A,H36B,
 H36C), C37A(H37A,H37B,H37C), C36B(H36D,H36E,H36F), C37B(H37D,H37E,H37F),
 C39A(H39A,H39B,H39C), C40A(H40A,H40B,H40C), C39B(H39D,H39E,H39F), C40B(H40D,
 H40E,H40F)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C26(H26), C24(H24), C47(H47), C45(H45)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C49(H49A,H49B,H49C), C34(H34A,
 H34B,H34C), C42(H42A,H42B,H42C), C51A(H51A,H51B,H51C), C52A(H52A,H52B,H52C),
 C51B(H51D,H51E,H51F), C52B(H52D,H52E,H52F), C63A(H63A,H63B,H63C), C63B(H63D,
 H63E,H63F)
;
_olex2_submission_special_instructions 'No special instructions were received'