{μ-6,6'-Diethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}trinitratoholmium(III)nickel(II)
Xiao, Yi-An; Fu, Xiang-Kai; Sui, Yan; Wu, Qing; Xiong, Shao-Hui; Acta Crystallographica Section E 64 (2008) m806–m807; doi:10.1107/S1600536808013755

data_2218429
_publ_section_title
{\m-6,6'-Diethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}trinitratoholmium(III)nickel(II)
_journal_coeditor_code           HG2401
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m806
_journal_page_last               m807
_journal_paper_doi               10.1107/S1600536808013755
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ho Ni (C20 H22 N2 O4) (N O3)3]'
_chemical_formula_moiety         'C20 H22 Ho N5 Ni O13'
_chemical_formula_sum            'C20 H22 Ho N5 Ni O13'
_chemical_formula_weight         764.07
_chemical_name_systematic
;{\m-6,6'-diethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato-
1\k^4^O^1^,<i>O</i>^1'^,<i>O</i>^6^,<i>O</i>^6'^:
2\k^4^O^1^,<i>N</i>,<i>N</i>',O^1'^'}trinitrato-1\k^6^O,<i>O</i>'-holmium(III)
nickel(II))
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5825(8)
_cell_length_b                   13.7028(14)
_cell_length_c                   21.203(2)
_cell_measurement_reflns_used    6504
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.92
_cell_volume                     2493.6(4)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'APEX2 (Bruker, 2004)'
_computing_molecular_graphics    'APEX2 (Bruker, 2004)'
_computing_publication_material
'APEX2 (Bruker, 2004) and publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18705
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    3.984
_exptl_absorpt_correction_T_max  0.6255
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.001
_refine_diff_density_min         -0.614
_refine_ls_abs_structure_details 'Flack (1983), 2455 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.003(18)
_refine_ls_extinction_coef       0.0058(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0473P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                4299
_reflns_number_total             5970
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2401.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2218429
_cod_database_fobs_code          2218429