Novel mixed-valence Cu compounds formed by Cu(II) dimers with double oximato bridges: in situ formation of anionic layer [Cu2(SCN)3]n(n-).
Dhal, Piu; Nandy, Madhusudan; Sadhukhan, Dipali; Zangrando, Ennio; Pilet, Guillaume; Gómez-García, Carlos J; Mitra, Samiran; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14545–14555; doi:10.1039/c3dt51561c

data_7023602
_publ_section_title
;
 Novel mixed-valence Cu compounds formed by Cu(II) dimers with double
 oximato bridges: in situ formation of anionic layer [Cu2(SCN)3]n(n-).
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14545
_journal_page_last               14555
_journal_paper_doi               10.1039/c3dt51561c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C16 H36 Cl2 Cu2 N6 O12'
_chemical_formula_sum            'C16 H36 Cl2 Cu2 N6 O12'
_chemical_formula_weight         702.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-07-13
_audit_creation_method           CRYSTALS_ver_14.21
_cell_angle_alpha                90
_cell_angle_beta                 90.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3445(2)
_cell_length_b                   12.0554(2)
_cell_length_c                   17.4604(3)
_cell_measurement_reflns_used    6647
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2808.91(8)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12528
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         29.152
_diffrn_reflns_theta_min         3.259
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1359
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.0005638
_refine_ls_shift/su_mean         0.0000190
_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: 
 23.2 31.0 20.7 14.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0703
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0638
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5625
_reflns_number_total             6257
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.95
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0585
_oxford_refine_ls_scale          3.007(9)
_oxford_reflns_number_all        6243
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ju449 in P 21/n'
_cod_data_source_file            c3dt51561c.txt
_cod_data_source_block           global
_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 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7023602
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.300000 , 0.010000 = CL(6) TO O(61) 
DISTANCE 1.300000 , 0.010000 = CL(6) TO O(62) 
DISTANCE 1.300000 , 0.010000 = CL(6) TO O(63) 
DISTANCE 1.300000 , 0.010000 = CL(6) TO O(64) 
DISTANCE 1.300000 , 0.010000 = CL(7) TO O(71) 
DISTANCE 1.300000 , 0.010000 = CL(7) TO O(72) 
DISTANCE 1.300000 , 0.010000 = CL(7) TO O(73) 
DISTANCE 1.300000 , 0.010000 = CL(7) TO O(74) 
U(IJ)'S  0.0, 0.010000 = O(21) TO CU(2) 
U(IJ)'S  0.0, 0.010000 = O(11) TO CU(1) 
U(IJ)'S  0.0, 0.010000 = CL(6) TO O(61) 
U(IJ)'S  0.0, 0.010000 = CL(6) TO O(62) 
U(IJ)'S  0.0, 0.010000 = CL(6) TO O(63) 
U(IJ)'S  0.0, 0.010000 = CL(6) TO O(64) 
U(IJ)'S  0.0, 0.010000 = CL(7) TO O(71) 
U(IJ)'S  0.0, 0.010000 = CL(7) TO O(72) 
U(IJ)'S  0.0, 0.010000 = CL(7) TO O(73) 
U(IJ)'S  0.0, 0.010000 = CL(7) TO O(74) 
END                                                                             
;