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_7206480
_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_formula_moiety
;
3(C21 H24 N2 Ni1 O4),K2,(C8 H20 N),(C6 Mo N6 S6),4(C2 H3 N), 2(H2 O)
;
_chemical_formula_sum            'C85 H108 K2 Mo N17 Ni3 O14 S6'
_chemical_formula_weight         2134.56
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.626(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3664(8)
_cell_length_b                   37.452(2)
_cell_length_c                   12.1573(8)
_cell_measurement_reflns_used    9586
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     10245.9(10)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.075
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48950
_diffrn_reflns_theta_full        28.715
_diffrn_reflns_theta_max         29.301
_diffrn_reflns_theta_min         2.829
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4420
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.80
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.0099963
_refine_ls_shift/su_mean         0.0000640
_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:
0.436 0.460 0.192
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1563
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0653
_reflns_limit_h_max              30
_reflns_limit_h_min              -32
_reflns_limit_k_max              51
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5635
_reflns_number_total             14120
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0639
_oxford_reflns_number_all        14088
_oxford_reflns_threshold_expression_ref I>1.8\s(I)
_cod_data_source_file            c1ce05127j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        10246.0(10)
_cod_original_sg_symbol_H-M      'C 1 2/m 1 '
_cod_original_formula_sum        'C85 H108 K2 Mo1 N17 Ni3 O14 S6'
_cod_database_code               7206480