Effect of Coordinating Solvents on the Structure of Cu(II)-4,4'-bipyridine Coordination Polymers
Rancan, M.; Carlotto, A.; Bottaro, G.; Armelao, L.; Inorganics 7 (2019) 103–; doi:10.3390/inorganics7080103

data_1556422
_publ_section_title
;
 Effect of Coordinating Solvents on the Structure of
 Cu(II)-4,4'-bipyridine Coordination Polymers
;
_journal_name_full               Inorganics
_journal_page_first              103
_journal_paper_doi               10.3390/inorganics7080103
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety
'0.5(C40 H40 Cu2 N8 O4), 2(Cl O4), 2(C4 H9 N O)'
_chemical_formula_sum            'C28 H38 Cl2 Cu N6 O12'
_chemical_formula_weight         785.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.562(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4924(10)
_cell_length_b                   11.1385(7)
_cell_length_c                   22.2237(13)
_cell_measurement_reflns_used    3458
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      26.6340
_cell_measurement_theta_min      2.9730
_cell_volume                     3586.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      301(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0637
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details
;
  1 omega  -25.00   30.00   0.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3052  -99.0000   60.0000 275

  2 omega  -58.00   42.00   0.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3052  -77.0000   90.0000 500

  3 omega  -58.00   42.00   0.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3052  -77.0000    0.0000 500

  4 omega   32.00   59.00   0.2000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.3052 -179.0000  -60.0000 135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0418026000
_diffrn_orient_matrix_UB_12      -0.0058627000
_diffrn_orient_matrix_UB_13      -0.0171315000
_diffrn_orient_matrix_UB_21      -0.0249338000
_diffrn_orient_matrix_UB_22      -0.0033946000
_diffrn_orient_matrix_UB_23      0.0269393000
_diffrn_orient_matrix_UB_31      -0.0052010000
_diffrn_orient_matrix_UB_32      0.0633398000
_diffrn_orient_matrix_UB_33      -0.0001232000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4544
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.650
_diffrn_reflns_theta_min         2.306
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1246P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3771
_reflns_number_total             4544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           3
_cod_database_code               1556422
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.611(2)
 0.389(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid body (RIGU) restrains
 O5, Cl1, O3, O6, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Free rotating group:
 O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C5(H5), C2(H2), C4(H4), C11(H11), C7(H7), C6(H6)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              38927
_shelx_hkl_checksum              93942