Synthesis and Aldol Reactivity of O- and C-Enolate Complexes of Nickel
Juan Cámpora; Celia M. Maya; Pilar Palma; Ernesto Carmona; Enrique Gutiérrez-Puebla; Caridad Ruiz; Journal of the American Chemical Society 125 (2003) 1482–1483; doi:10.1021/ja028711f

data_4113449
_publ_contact_author
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        Caridad Ruiz-Valero
        Instituto de Ciencia de Materiales
        CSIC
        Campus de Cantoblanco
        28049 MADRID
        Spain
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_publ_contact_author_email       crvalero@icmm.csic.es
_publ_contact_author_fax         '34 1 372-0623'
_publ_contact_author_phone       '34 1 334-9026'
_publ_section_title
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 Synthesis and Aldol Reactivity of O- and C-Enolate Complexes of Nickel
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1482
_journal_page_last               1483
_journal_paper_doi               10.1021/ja028711f
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C22 H38 Ni O P2'
_chemical_formula_weight         439.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 116.966(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.717(4)
_cell_length_b                   12.898(2)
_cell_length_c                   19.394(3)
_cell_measurement_temperature    148(2)
_cell_volume                     4618.8(14)
_computing_cell_refinement       'Siemens SAINT (Bruker)'
_computing_data_collection       'Siemens SMART (Bruker)'
_computing_data_reduction        'Siemens SAINT (Bruker)'
_computing_molecular_graphics    'Siemens-Bruker SHELXTL'
_computing_publication_material  'Siemens-Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      148(2)
_diffrn_measurement_device       'Siemens-Bruker SMART CCD'
_diffrn_measurement_method       '\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  0.1608
_diffrn_reflns_av_sigmaI/netI    0.2530
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7855
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.968
_refine_ls_goodness_of_fit_obs   1.164
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.2071
_refine_ls_R_factor_obs          0.0898
_refine_ls_shift/esd_max         1.269
_refine_ls_shift/esd_mean        0.127
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1853
_refine_ls_wR_factor_obs         0.1428
_reflns_number_observed          1881
_reflns_number_total             4030
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja028711f-2_s2.cif
_cod_data_source_block           R168
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4618.6(14)
_cod_database_code               4113449