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_1556425
_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         'C20 H34 Cu N4 O4 S2, 2(Cl O4)'
_chemical_formula_sum            'C20 H34 Cl2 Cu N4 O12 S2'
_chemical_formula_weight         721.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 100.154(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9524(17)
_cell_length_b                   11.0913(7)
_cell_length_c                   16.3512(15)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    299.6(6)
_cell_measurement_theta_max      27.3020
_cell_measurement_theta_min      2.4620
_cell_volume                     3204.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      299.6(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1274
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -54.00  44.00   0.50   10.00    --   18.52 -38.00 150.00  196
  2  \w    -52.00  49.00   0.50   10.00    --   18.52 -77.00 -90.00  202
  3  \w    -12.00  89.00   0.50   10.00    --   18.52  77.00  30.00  202
  4  \w    -26.00  91.00   0.50   10.00    --   18.52  19.00 -60.00  234
  5  \w    -73.00 -35.00   0.50   10.00    --  -18.60 121.00   0.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0049725000
_diffrn_orient_matrix_UB_12      0.0484797000
_diffrn_orient_matrix_UB_13      -0.0286476000
_diffrn_orient_matrix_UB_21      0.0004615000
_diffrn_orient_matrix_UB_22      -0.0411596000
_diffrn_orient_matrix_UB_23      -0.0331333000
_diffrn_orient_matrix_UB_31      -0.0398572000
_diffrn_orient_matrix_UB_32      -0.0066054000
_diffrn_orient_matrix_UB_33      -0.0046070000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13522
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       needle
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0426P)^2^+3.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2795
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6.cif
_cod_data_source_block           6
_cod_database_code               1556425
_chemical_oxdiff_formula         'Cu1 N2 C10 H10 Cl2 O8'
_chemical_oxdiff_usercomment
'cristallo azzurro chiaro da MR100, dopo un mese, DMF+ DMSO vap Et2O'
_reflns_odcompleteness_completeness 99.91
_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. Restrained distances
 O6B-O3B \\sim O6B-O4B \\sim O6B-O5B \\sim O4A-O5A \\sim O4A-O3A \\sim O4A-O6A
\\sim O5A-O3A
 with sigma of 0.04
 Cl1-O6B \\sim Cl1-O4A \\sim Cl1-O5A \\sim Cl1-O3B \\sim Cl1-O3A \\sim Cl1-O4B
\\sim Cl1-O6A \\sim Cl1-O5B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O4A, Cl1, O6B, O4B, O3B, O5A, O6A, O3A, O5B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O5B)=Sof(O6B)=Sof(O4B)=Sof(O3B)=1-FVAR(1)
 Sof(O6A)=Sof(O3A)=Sof(O5A)=Sof(O4A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C9(H9), C5(H5), C6(H6)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              98099
_shelx_hkl_checksum              2544
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.839