Oligomeric and polymeric organizations of potassium salts with compartmental Schiff-base complexes as ligands
Mousavi, Maliheh; Béreau, Virginie; Costes, Jean-Pierre; Duhayon, Carine; Sutter, Jean-Pascal; CrystEngComm 13 (2011) 5908–; doi:10.1039/c1ce05127j

data_7206483
_publ_section_title
;
 Oligomeric and polymeric organizations of potassium salts with
 compartmental Schiff-base complexes as ligands
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              5908
_journal_paper_doi               10.1039/c1ce05127j
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H47 K1 N4 Ni2 O10'
_chemical_formula_sum            'C40 H47 K N4 Ni2 O10'
_chemical_formula_weight         900.36
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.190(9)
_cell_length_b                   18.190(9)
_cell_length_c                   11.780(5)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    110
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3376(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.084
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            65962
_diffrn_reflns_theta_full        28.011
_diffrn_reflns_theta_max         28.583
_diffrn_reflns_theta_min         1.293
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1401
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.73
_refine_ls_abs_structure_details 'Flack (1983), 2576 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0862
_refine_ls_shift/su_max          0.0002136
_refine_ls_shift/su_mean         0.0000109
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.26 1.17 1.62
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1274
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0859
_reflns_limit_h_max              12
_reflns_limit_h_min              -24
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4037
_reflns_number_total             5715
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0797
_oxford_reflns_number_all        5696
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c1ce05127j.txt
_cod_data_source_block           cpd1102
_cod_original_sg_symbol_Hall     'P 31 2" '
_cod_original_sg_symbol_H-M      'P 31 2 1 '
_cod_original_formula_sum        'C40 H47 K1 N4 Ni2 O10'
_cod_database_code               7206483