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_1556423
_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(C52 H60 Cu2 N12 O4), 2(Cl O4), 2(C10 H8 N2)'
_chemical_formula_sum            'C46 H46 Cl2 Cu N10 O10'
_chemical_formula_weight         1033.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 106.641(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2921(4)
_cell_length_b                   15.7544(4)
_cell_length_c                   15.3205(5)
_cell_measurement_reflns_used    7831
_cell_measurement_temperature    301(3)
_cell_measurement_theta_max      29.0590
_cell_measurement_theta_min      2.4780
_cell_volume                     2380.11(14)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      301(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   -3.00   87.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219   57.0000 -120.0000 360

  2 omega  -50.00   40.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  -57.0000  120.0000 360

  3 omega  -25.00   23.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6000  -99.0000  -60.0000 192

  4 omega  -89.00   11.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6000  -77.0000    0.0000 400

  5 omega   34.00   59.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5219  179.0000  120.0000 100

  6 omega  -44.00   54.00   0.2500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6000   38.0000  -30.0000 392
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0435605000
_diffrn_orient_matrix_UB_12      -0.0288499000
_diffrn_orient_matrix_UB_13      -0.0134648000
_diffrn_orient_matrix_UB_21      -0.0297973000
_diffrn_orient_matrix_UB_22      -0.0342177000
_diffrn_orient_matrix_UB_23      0.0174309000
_diffrn_orient_matrix_UB_31      -0.0489602000
_diffrn_orient_matrix_UB_32      -0.0048702000
_diffrn_orient_matrix_UB_33      -0.0429789000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19893
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.315
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84772
_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            'dark blue'
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4830
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0480P)^2^+1.0563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4256
_reflns_number_total             4830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           4
_cod_database_code               1556423
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C11(H11), C9(H9), C2(H2), C4(H4), C3(H3), C10(H10), C8(H8), C7(H7),
 C16(H16), C21(H21), C17(H17), C15(H15), C20(H20), C22(H22), C23(H23), C14(H14)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              94448
_shelx_hkl_checksum              73659
_olex2_submission_special_instructions 'No special instructions were received'