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_7700601
_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         'C25 H23 Cu N3 O2'
_chemical_formula_sum            'C25 H23 Cu N3 O2'
_chemical_formula_weight         461.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-28
_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                90
_cell_angle_beta                 90.788(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2782(4)
_cell_length_b                   18.5496(7)
_cell_length_c                   12.2910(4)
_cell_measurement_reflns_used    13635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5040
_cell_measurement_theta_min      2.0440
_cell_volume                     2115.17(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.965
_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   -107.00  73.00   1.00   10.00    --  -17.00   8.00 -50.00  180
  2  \w   -106.00  22.00   1.00   10.00    --  -17.00 -72.00  49.00  128
  3  \w    -87.00  22.00   1.00   10.00    --  -17.00 -72.00-148.00  109
  4  \w    -30.00  -3.00   1.00   10.00    --  -17.00  72.00 -17.00   27
  5  \w    -27.00 -12.00   1.00   10.00    --  -17.00  24.00-148.00   15
  6  \w     37.00  53.00   1.00   10.00    --  -17.00   8.00 -17.00   16
  7  \w   -107.00 -24.00   1.00   10.00    --  -17.00  -8.00-180.00   83
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0647377000
_diffrn_orient_matrix_UB_12      0.0143135000
_diffrn_orient_matrix_UB_13      -0.0224372000
_diffrn_orient_matrix_UB_21      0.0382096000
_diffrn_orient_matrix_UB_22      0.0120752000
_diffrn_orient_matrix_UB_23      -0.0461194000
_diffrn_orient_matrix_UB_31      -0.0140134000
_diffrn_orient_matrix_UB_32      -0.0333296000
_diffrn_orient_matrix_UB_33      -0.0264580000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27288
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.657
_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    1.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71943
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0379P)^2^+0.6320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                7698
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           2016tdk012
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_original_cell_volume        2115.16(14)
_cod_database_code               7700601
_chemical_oxdiff_formula         (CuC13H9N1O2)(C6H7N)2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.970(4) 0.030(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
N111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim
N121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim C147 \\sim
N151 \\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156 \\sim C157: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N111, C112, C113, C114, C115, C116, C117, N121, C122, C123, C124, C125, C126,
 C127
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N141, C142, C143, C144, C145, C146, C147, N151, C152, C153, C154, C155, C156,
 C157
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N111, C112, C113, C114, C115, C116, C117} sigma for 1-2: 0.02, 1-3: 0.04
as
{N121, C122, C123, C124, C125, C126, C127}
{N141, C142, C143, C144, C145, C146, C147} sigma for 1-2: 0.02, 1-3: 0.04
as
{N151, C152, C153, C154, C155, C156, C157}
6. Others
 Sof(N121)=Sof(C122)=Sof(H122)=Sof(C123)=Sof(C124)=Sof(H124)=Sof(C125)=
 Sof(H125)=Sof(C126)=Sof(H126)=Sof(C127)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(1)
 Sof(N111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(C114)=Sof(H114)=Sof(C115)=
 Sof(H115)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Sof(N151)=Sof(C152)=Sof(H152)=Sof(C153)=Sof(C154)=Sof(H154)=Sof(C155)=
 Sof(H155)=Sof(C156)=Sof(H156)=Sof(C157)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(2)
 Sof(N141)=Sof(C142)=Sof(H142)=Sof(C143)=Sof(C144)=Sof(H144)=Sof(C145)=
 Sof(H145)=Sof(C146)=Sof(H146)=Sof(C147)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
7.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), C102(H102), C104(H104), C105(H105), C106(H106), C112(H112),
  C114(H114), C115(H115), C116(H116), C122(H122), C124(H124), C125(H125),
 C126(H126), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C61(H61),
 C62(H62), C63(H63), C64(H64), C132(H132), C134(H134), C135(H135), C136(H136),
 C142(H142), C144(H144), C145(H145), C146(H146), C152(H152), C154(H154),
 C155(H155), C156(H156)
7.b Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C117(H11A,H11B,H11C), C127(H12A,H12B,H12C), C137(H13A,
 H13B,H13C), C147(H14A,H14B,H14C), C157(H15A,H15B,H15C)
;
_shelx_res_checksum              93255
_shelx_shelxl_version_number     2014/7
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.541
_oxdiff_exptl_absorpt_empirical_full_min 0.482