Synthesis, characterization, and unique catalytic activities of a fluorinated nickel enolate.
Doi, Ryohei; Kikushima, Kotaro; Ohashi, Masato; Ogoshi, Sensuke; Journal of the American Chemical Society 137 (2015) 3276–3282; doi:10.1021/ja511730k

data_4123482
_publ_section_title
;
 Synthesis, characterization, and unique catalytic activities of a
 fluorinated nickel enolate.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3276
_journal_page_last               3282
_journal_paper_doi               10.1021/ja511730k
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C49 H63 F2 Ni O2 P2, C18 B F16'
_chemical_formula_sum            'C67 H63 B F18 Ni O2 P2'
_chemical_formula_weight         1373.63
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.5800(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7131(2)
_cell_length_b                   19.5556(4)
_cell_length_c                   28.4483(5)
_cell_measurement_reflns_used    57533
_cell_measurement_temperature    123(2)
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_cell_measurement_theta_min      3.11
_cell_volume                     6515.9(2)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'Sir2011 (M.C.Burla, et al., 2012)'
_computing_molecular_graphics    'CrystalMaker (CrystalMaker Software Ltd,)'
_computing_publication_material  'SHELXL-2013 and modified'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Sir2011 (M.C.Burla, et al., 2012)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            100752
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.107
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1999). Abscor - Empirical Absorption Correction based on
Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       needle
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0042(3)
_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   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         11568
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1724P)^2^+6.6994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2696
_refine_ls_wR_factor_ref         0.3413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5900
_reflns_number_total             11568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja511730k_si_001.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/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 3086 2015-02-26 13:12:21Z robertas 

 Adding full bibliography for 4123479--4123482.cif.
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_cod_database_code               4123482
_shelx_estimated_absorpt_t_min   0.846
_shelx_estimated_absorpt_t_max   0.846
_shelxl_version_number           2013-4
_shelx_res_checksum              45032
_shelx_hkl_checksum              54841
_shelx_fab_checksum              8449