All about that base: investigating the role of ligand basicity in pyridyl complexes derived from a copper-Schiff base coordination polymer.
Beddoe, Samuel V. F.; Lonergan, Rhona F.; Pitak, Mateusz B.; Price, Jason R.; Coles, Simon J.; Kitchen, Jonathan A.; Keene, Tony D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15553–15559; doi:10.1039/c9dt01527b

data_7700603
_publ_section_title
;
 All about that base: investigating the role of ligand basicity in pyridyl
 complexes derived from a copper-Schiff base coordination polymer.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15553
_journal_page_last               15559
_journal_paper_doi               10.1039/c9dt01527b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C19 H17 Cu N3 O4, C2 H6 O S'
_chemical_formula_sum            'C21 H23 Cu N3 O5 S'
_chemical_formula_weight         493.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2019-04-01 deposited with the CCDC.    2019-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                68.148(5)
_cell_angle_beta                 81.123(4)
_cell_angle_gamma                88.371(4)
_cell_formula_units_Z            2
_cell_length_a                   5.6328(2)
_cell_length_b                   12.7929(6)
_cell_length_c                   15.6440(9)
_cell_measurement_reflns_used    9531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4840
_cell_measurement_theta_min      1.7730
_cell_volume                     1033.26(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_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_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -30.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000   72.0000   30.0000 104

  2 omega  -67.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000  -72.0000  -90.0000 90

  3 omega  -63.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000  -72.0000   90.0000 86

  4 omega  -87.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000    0.0000  -90.0000 77

  5 omega  -39.00  -24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000   72.0000 -120.0000 15

  6 omega -106.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000    0.0000    0.0000 180
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_UB_11      -0.0284859000
_diffrn_orient_matrix_UB_12      0.0200151000
_diffrn_orient_matrix_UB_13      0.0368731000
_diffrn_orient_matrix_UB_21      0.1198156000
_diffrn_orient_matrix_UB_22      0.0211662000
_diffrn_orient_matrix_UB_23      -0.0081885000
_diffrn_orient_matrix_UB_31      -0.0330498000
_diffrn_orient_matrix_UB_32      0.0521870000
_diffrn_orient_matrix_UB_33      -0.0319110000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13694
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) 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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       needle
_exptl_crystal_F_000             510
_exptl_crystal_recrystallization_method
'Crystallisation by slow diffusion of water vapour into DMSO solution'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     718
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0243P)^2^+0.9792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4098
_reflns_number_total             4701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           bus_test1
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_original_cell_volume        1033.26(10)
_cod_database_code               7700603
_chemical_oxdiff_formula         (C13H9N1O2Cu1)(C6H6N2O1)
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O27-H27A = O27-H27B
 0.88 with sigma of 0.01
 H27A-H27B
 1.4 with sigma of 0.01
3. Restrained planarity
 C32, C33, C34, C35, C36, C37
 with sigma of 0.1
 C40, C41, C42, C43, C44, C45
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cu1 \\sim O11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim
N18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim
O26 \\sim O27 \\sim Cu2 \\sim O31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim N38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim
C44 \\sim C45 \\sim O46 \\sim O47: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(Cu1) = Uanis(Cu2)
5. Rigid body (RIGU) restrains
 Cu1, O11, C12, C13, C14, C15, C16, C17, N18, C19, C20, C21, C22, C23, C24,
 C25, O26, O27, Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42,
  C43, C44, C45, O46, O47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{Cu1, O11, C12, C13, C14, C15, C16, C17, N18, C19, C20, C21, C22, C23, C24,
C25, O26, O27} sigma for 1-2: 0.002, 1-3: 0.004
as
{Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42, C43, C44,
C45, O46, O47}
7. Others
 Sof(Cu2)=Sof(O31)=Sof(C32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(N38)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=
 Sof(C45)=Sof(O46)=Sof(O47)=1-FVAR(1)
 Sof(Cu1)=Sof(O11)=Sof(C12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(N18)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=
 Sof(C25)=Sof(O26)=Sof(O27)=FVAR(1)
 Uiso(O31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=Uiso(C37)=
 Uiso(N38)=Uiso(C39)=Uiso(C40)=Uiso(C41)=Uiso(C42)=Uiso(C43)=Uiso(C44)=
 Uiso(C45)=Uiso(O46)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C21(H21), C22(H22),
 C23(H23), C24(H24), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C41(H41),
  C42(H42), C43(H43), C44(H44), C52(H52), C53(H53), C55(H55), C56(H56)
8.b X=CH2 refined with riding coordinates:
 N59(H59A,H59B)
8.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              89763
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method Mitegen
_olex2_submission_special_instructions 'No special instructions were received'