Tetraaquabis{μ~2~-2,7-bis[(2,6-diisopropylphenyl)iminomethyl]naphthalene-1,8-diolato}di-μ~3~-hydroxido-di-μ~2~-hydroxido-bis(trimethylphosphine oxide)tetranickel(II)‒trimethylphosphine oxide‒diethyl ether‒water (1/2/2/2)
Delferro, Massimiliano; Weberski, Jr, Michael P.; Rodriguez, Brandon A.; Marks, Tobin J.; Acta Crystallographica Section E 66 (2010) m257–; doi:10.1107/S1600536810003697

data_2225359
_publ_section_title
;Tetraaquabis{\m~2~-2,7-bis[(2,6-diisopropylphenyl)iminomethyl]naphthalene-1,8-diolato}di-\m~3~-hydroxido-di-\m~2~-hydroxido-bis(trimethylphosphine
 oxide)tetranickel(II)--trimethylphosphine oxide--diethyl ether--water
 (1/2/2/2)
;
_journal_coeditor_code           RZ2413
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m257
_journal_paper_doi               10.1107/S1600536810003697
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
;
[Ni4 (C36 H40 N2 O2)2 (O H)4 (C3 H9 O P)2 (H2 O)4],
2C4 H10 O, 2C3 H9 O P, 2H2 O
;
_chemical_formula_moiety
'C78 H110 N4 Ni4 O14 P2, 2(C4 H10 O), 2(C3 H9 O P), 2(H2 O)'
_chemical_formula_sum            'C92 H152 N4 Ni4 O20 P4'
_chemical_formula_weight         1992.90
_chemical_name_systematic
;Tetraaquabis{\m~2~-2,7-bis[(2,6-diisopropylphenyl)iminomethyl]naphthalene-1,8-
diolato}di-\m~3~-hydroxido-di-\m~2~-hydroxido-bis(trimethylphosphine
oxide)tetranickel(II)--trimethylphosphine
 oxide--diethyl ether--water (1/2/2/2)
;
_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                78.1090(10)
_cell_angle_beta                 72.7590(10)
_cell_angle_gamma                83.7820(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9818(2)
_cell_length_b                   13.7937(2)
_cell_length_c                   16.2215(3)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.94
_cell_measurement_theta_min      5.71
_cell_volume                     2502.37(7)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27203
_diffrn_reflns_theta_full        67.31
_diffrn_reflns_theta_max         67.31
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    1.986
_exptl_absorpt_correction_T_max  0.8984
_exptl_absorpt_correction_T_min  0.7867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.888
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         8609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                6279
_reflns_number_total             8609
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2413.cif
_cod_data_source_block           I
_cod_database_code               2225359
_cod_database_fobs_code          2225359