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_7701939
_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_formula_moiety
'0.25(C56 H32 Cu4 N8 O16), 0.5(H1.08 O), 1.5(H2 O)'
_chemical_formula_sum            'C14 H12 Cu N2 O6'
_chemical_formula_weight         367.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.932(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.503(3)
_cell_length_b                   17.141(3)
_cell_length_c                   8.8358(13)
_cell_measurement_reflns_used    1409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.308
_cell_measurement_theta_min      2.203
_cell_volume                     2800.8(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5505
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.047
_diffrn_reflns_theta_min         1.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.595
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0713 before and 0.0545 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0928 before and 0.0658 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 33237 reflections, Rint = 0.0944
 (9403 with I > 3sig(I), Rint = 0.0708)
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol, water'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.521
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5505
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      5.907
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+10.3995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4161
_reflns_number_total             5505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02417k2.cif
_cod_data_source_block           4844
_cod_original_cell_volume        2800.8(7)
_cod_database_code               7701939
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.664
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.703(2)
 0.297(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1W-H1WB = O1W-H1WA = O2W-H2WA = O2W-H2WB = O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.01
 O3W-H3WB = O3W-H3WA
 0.8 with sigma of 0.001
4. Others
 Sof(H1WA)=Sof(H1WB)=FVAR(1)
5.a Everything fixed:
 O1W, H1WA, H1WB
5.b Free rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C10(H10), C11(H11), C17(H17),
 C18(H18), C21(H21), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28)
;
_olex2_submission_special_instructions 'No special instructions were received'