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_7700611
_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         'C18 H15 Cu N3 O2'
_chemical_formula_sum            'C18 H15 Cu N3 O2'
_chemical_formula_weight         368.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-06
_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                 90.0016(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.51709(13)
_cell_length_b                   5.49923(6)
_cell_length_c                   17.54359(16)
_cell_measurement_reflns_used    78789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.9200
_cell_measurement_theta_min      2.3210
_cell_volume                     1497.03(2)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -119.00   35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000    0.0000  150.0000 308

  2 omega  -68.00   61.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000   72.0000  120.0000 258

  3 omega  -65.50    8.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000    0.0000  -90.0000 147

  4 omega  -57.50    9.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000  -72.0000   90.0000 133

  5 omega  -65.00   61.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000   54.0000  120.0000 252

  6 omega -119.00  -65.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.0000    0.0000 -180.0000 108

  7 omega  -86.00    3.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000  150.0000 178

  8 omega -174.00  -68.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -54.0000   60.0000 212

  9 omega  -92.50  -32.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   54.0000  -60.0000 121

 10 omega -139.00 -118.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   18.0000 -180.0000 42

 11 omega -122.00 -102.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000    0.0000  -30.0000 40

 12 omega -177.00  -26.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -18.0000  -60.0000 302

 13 omega -109.00    2.50   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000 -180.0000 223

 14 omega  -81.50    3.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000   90.0000 169

 15 omega -140.00 -105.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   18.0000 -150.0000 70

 16 omega -115.00    1.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000 -120.0000 232

 17 omega -106.00  -65.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   54.0000  120.0000 82

 18 omega -117.00  -96.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000 -150.0000 42

 19 omega  -69.00  -48.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -72.0000   60.0000 42

 20 omega -113.50   -8.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   54.0000  150.0000 211

 21 omega -149.00  -51.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -54.0000 -120.0000 196

 22 omega -162.00  -26.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -18.0000  -90.0000 272

 23 omega  -91.00    2.50   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   54.0000 -150.0000 187

 24 omega -141.50  -48.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -72.0000   30.0000 187

 25 omega -123.50  -48.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -72.0000   90.0000 151

 26 omega -126.00  -19.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000  120.0000 214

 27 omega -148.50  -61.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -18.0000   60.0000 175

 28 omega  -99.50  -61.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   54.0000 -180.0000 77

 29 omega  -69.00  -48.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -72.0000  120.0000 42

 30 omega  -64.00  -43.50   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000   72.0000   60.0000 41

 31 omega  -71.00  -51.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -54.0000   30.0000 40

 32 omega -146.00    3.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000    0.0000 -150.0000 298

 33 omega -177.00 -137.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -87.0000  -72.0000    0.0000 80
;
_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      -0.0031036000
_diffrn_orient_matrix_UB_12      0.0059752000
_diffrn_orient_matrix_UB_13      -0.0402901000
_diffrn_orient_matrix_UB_21      -0.0161384000
_diffrn_orient_matrix_UB_22      -0.1206832000
_diffrn_orient_matrix_UB_23      -0.0007977000
_diffrn_orient_matrix_UB_31      -0.0426515000
_diffrn_orient_matrix_UB_32      0.0451804000
_diffrn_orient_matrix_UB_33      0.0032250000
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            211441
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         62.632
_diffrn_reflns_theta_min         1.752
_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    1.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       slab
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         24013
_refine_ls_number_restraints     316
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18849
_reflns_number_total             24013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           tdk-sn2-052a_fullhigh
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_database_code               7700611
_chemical_oxdiff_formula         'C18 H15 N3 O2 Cu'
_reflns_odcompleteness_completeness 98.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.41
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99862(13) 0.00138(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Uiso/Uaniso restraints and constraints
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: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42, C43, C44,
 C45, O46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Cu1, O11, C12, C13, C14, C15, C16, C17, N18, C19, C20, C21, C22, C23, C24,
C25, O26} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42, C43, C44,
C45, O46}
6. 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)=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)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C55(H55), C56(H56), 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)
7.b X=CH2 refined with riding coordinates:
 N57(H57A,H57B)
;
_shelx_res_checksum              25688
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'