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_7023604
_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         'C77 H80 Cu5 N17 O4 S5'
_chemical_formula_sum            'C77 H80 Cu5 N17 O4 S5'
_chemical_formula_weight         1785.65
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90.0
_cell_angle_beta                 115.620(10)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   51.203(4)
_cell_length_b                   12.5267(7)
_cell_length_c                   29.582(3)
_cell_measurement_reflns_used    4501
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     17109(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.778
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36747
_diffrn_reflns_theta_full        18.701
_diffrn_reflns_theta_max         24.935
_diffrn_reflns_theta_min         2.995
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.403
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7344
_exptl_crystal_size_max          0.686
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.063
_platon_squeeze_details
;
;
_refine_diff_density_max         2.18
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1115
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         9292
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.0006761
_refine_ls_shift/su_mean         0.0000151
_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: 
 1.94 -2.66 -0.187 -1.50 -0.746 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1308
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0931
_reflns_limit_h_max              53
_reflns_limit_h_min              -56
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                7504
_reflns_number_total             11614
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.77
_oxford_diffrn_Wilson_scale      45.75
_oxford_refine_ls_r_factor_ref   0.1072
_oxford_refine_ls_scale          0.1598(3)
_oxford_reflns_number_all        11601
_oxford_reflns_threshold_expression_ref I>1.0\s(I)
_cod_data_source_file            c3dt51561c.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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 

2018-03-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C154 H160 Cu10 N34 O8 S10'
_cod_original_formula_weight         3571.31
_cod_original_formula_moiety         'C154 H160 Cu10 N34 O8 S10'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        17109(2)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7023604
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
FIX C(43,U'S) UNTIL C(46) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.001000 = C(5) TO C(6) 
U(IJ)'S  0.0, 0.010000 = C(6) TO N(3) 
U(IJ)'S  0.0, 0.010000 = C(201) TO C(93) 
DISTANCE 1.350000 , 0.020000 = C(44) TO C(45) 
DISTANCE 1.350000 , 0.050000 = C(45) TO C(46) 
END                                                                             
;