Synthesis and Reactivity of Four- and Five-Coordinate Low-Spin Cobalt(II) PCP Pincer Complexes and Some Nickel(II) Analogues
Murugesan, Sathiyamoorthy; Stöger, Berthold; Carvalho, Maria Deus; Ferreira, Liliana P.; Pittenauer, Ernst; Allmaier, Günter; Veiros, Luis F.; Kirchner, Karl; Organometallics  (2014) 141009125933001–; doi:10.1021/om5007769

data_4084480
_publ_section_title
;
 Synthesis and Reactivity of Four- and Five-Coordinate Low-Spin Cobalt(II)
 PCP Pincer Complexes and Some Nickel(II) Analogues
;
_journal_name_full               Organometallics
_journal_page_first              141009125933001
_journal_paper_doi               10.1021/om5007769
_journal_year                    2014
_chemical_formula_sum            'C20 H37 Cl Co N2 P2'
_chemical_formula_weight         461.9
_chemical_name_systematic        ' ?'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.829(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.566(3)
_cell_length_b                   11.279(2)
_cell_length_c                   14.640(3)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.8
_cell_measurement_theta_min      2.3
_cell_volume                     2314.0(8)
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81191
_diffrn_reflns_theta_full        32.93
_diffrn_reflns_theta_max         33.06
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.3253
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details
'  7701 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.038(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.47
_refine_ls_goodness_of_fit_ref   1.39
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    298
_refine_ls_number_parameters     472
_refine_ls_number_reflns         81161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.0297
_refine_ls_shift/su_mean         0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0004F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                68052
_reflns_number_total             81161
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            om5007769_si_001.cif
_cod_data_source_block           CoCl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_cell_volume        2314.1(7)
_cod_original_formula_sum        'C20 H37 Cl1 Co1 N2 P2'
_cod_database_code               4084480