Effect of temperature and ligand protonation on the electronic ground state in Cu(ii) polymers having unusual secondary interactions: a magnetic and catechol oxidase study.
Saha, Sandeepta; Biswas, Niladri; Sasmal, Ashok; Gómez-García, Carlos J; Garribba, Eugenio; Bauza, Antonio; Frontera, Antonio; Pilet, Guillaume; Rosair, Georgina M.; Mitra, Samiran; Roy Choudhury, Chirantan; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16102–16118; doi:10.1039/c8dt02417k

data_7701938
_publ_section_title
;
 Effect of temperature and ligand protonation on the electronic ground
 state in Cu(ii) polymers having unusual secondary interactions: a
 magnetic and catechol oxidase study.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16102
_journal_page_last               16118
_journal_paper_doi               10.1039/c8dt02417k
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H12 Cu1 N3 O8.50'
_chemical_formula_sum            'C14 H12 Cu N3 O8.5'
_chemical_formula_weight         421.81
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2017-07-08 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3230(7)
_cell_length_b                   14.3515(6)
_cell_length_c                   7.4141(4)
_cell_measurement_reflns_used    5805
_cell_measurement_temperature    293
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     1630.42(13)
_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 0.979
_diffrn_measured_fraction_theta_max 0.904
_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  0.020
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9821
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         29.464
_diffrn_reflns_theta_min         2.839
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.598
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details 'Flack (1983), 1445 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.001(13)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0460
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0067930
_refine_ls_shift/su_mean         0.0002714
_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: 
 4.07 -0.968 2.18 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0334
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0328
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              -9
_reflns_number_gt                3338
_reflns_number_total             3548
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0324
_oxford_refine_ls_scale          3.006(4)
_oxford_reflns_number_all        3538
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c8dt02417k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C14 H12 Cu1 N3 O8.50'
_cod_database_code               7701938
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE O   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE O   (  41,X'S) H   (   1,X'S) H   (   2,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;