Synthesis and Reactivity of Nickel(II) Hydroxycarbonyl Species, NiCOOH-κC
Yoo, Changho; Kim, Jin; Lee, Yunho; Organometallics 32 (2013) 7195–; doi:10.1021/om400881j

data_4082001
_publ_section_title
;
 Synthesis and Reactivity of Nickel(II) Hydroxycarbonyl Species,
 NiCOOH-\kC
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7195
_journal_paper_doi               10.1021/om400881j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'Ni2C52H80N2O2P4, C4H10O1'
_chemical_formula_sum            'C57 H90 N2 Ni2 O3 P4'
_chemical_formula_weight         1092.61
_chemical_name_common            (PNP)NiCOONi(PNP)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                62.16(3)
_cell_angle_beta                 67.70(3)
_cell_angle_gamma                70.62(3)
_cell_formula_units_Z            2
_cell_length_a                   13.801(3)
_cell_length_b                   15.714(3)
_cell_length_c                   16.722(3)
_cell_measurement_reflns_used    84882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      0.36
_cell_volume                     2913.4(14)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.63000
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26892
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9739
_exptl_absorpt_correction_T_min  0.8154
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0259(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         13691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0890P)^2^+1.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                11697
_reflns_number_total             13691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400881j_si_002.cif
_cod_data_source_block           p27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2913.5(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082001