Formation of a tetranickel octacarbonyl cluster from the CO2 reaction of a zero-valent nickel monocarbonyl species
Yoo, Changho; Lee, Yunho; Inorganic Chemistry Frontiers 3 (2016) 849–; doi:10.1039/C6QI00011H

data_4349454
_publ_section_title
;
 Formation of a tetranickel octacarbonyl cluster from the CO2 reaction of
 a zero-valent nickel monocarbonyl species
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              849
_journal_paper_doi               10.1039/C6QI00011H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C70 H112 N2 Na2 Ni2 O8 P4'
_chemical_formula_sum            'C70 H112 N2 Na2 Ni2 O8 P4'
_chemical_formula_weight         1396.90
_chemical_name_common            {(PNP)NiCOONa}2(THF)
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_audit_update_record
;
2016-01-12 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                101.8930(10)
_cell_angle_beta                 96.7630(10)
_cell_angle_gamma                96.9260(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9465(3)
_cell_length_b                   12.3880(3)
_cell_length_c                   14.3038(4)
_cell_measurement_reflns_used    34833
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      0.9140
_cell_measurement_theta_min      0.8970
_cell_volume                     1863.77(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34833
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.82
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         16891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                13256
_reflns_number_total             16891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00011h2.cif
_cod_data_source_block           0063a-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/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 

2024-02-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C35 H56 N Na Ni O4 P2'
_cod_original_formula_weight         698.45
_cod_original_formula_moiety         'C35 H56 N Na Ni O4 P2'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4349454