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_7700613
_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 H14 Cu N2 O2'
_chemical_formula_sum            'C18 H14 Cu N2 O2'
_chemical_formula_weight         353.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7594(4)
_cell_length_b                   11.4338(3)
_cell_length_c                   13.2116(5)
_cell_measurement_reflns_used    10138
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4910
_cell_measurement_theta_min      2.3390
_cell_volume                     1474.24(9)
_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       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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    'SIR2011 (Burla 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 1.000
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -32.00 74.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 72.0000 100.0000 106 #__ type_ start__ end____ width___ exp.time_ 2 omega -70.00 23.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 -72.0000 -20.0000 93 #__ type_ start__ end____ width___ exp.time_ 3 omega -79.00 23.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 -72.0000 -180.0000 102 #__ type_ start__ end____ width___ exp.time_ 4 omega -96.00 -24.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 0.0000 -180.0000 72 #__ type_ start__ end____ width___ exp.time_ 5 omega -106.00 58.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 0.0000 -100.0000 164 #__ type_ start__ end____ width___ exp.time_ 6 omega -79.00 -61.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -16.0000 -72.0000 60.0000 18'
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  Kat
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_UB_11      -0.0186035000
_diffrn_orient_matrix_UB_12      -0.0579740000
_diffrn_orient_matrix_UB_13      0.0132412000
_diffrn_orient_matrix_UB_21      0.0650955000
_diffrn_orient_matrix_UB_22      -0.0082863000
_diffrn_orient_matrix_UB_23      0.0228182000
_diffrn_orient_matrix_UB_31      -0.0263985000
_diffrn_orient_matrix_UB_32      0.0204811000
_diffrn_orient_matrix_UB_33      0.0467634000
_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  0.0797
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18404
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.356
_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    1.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70108
_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.'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       needle
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 998 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3367
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0478P)^2^+0.2234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                2736
_reflns_number_total             3367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           2015tdk064
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_database_code               7700613
_chemical_oxdiff_formula         (C11H9NO2)Cu(C5H5N)
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. 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 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
3. Rigid body (RIGU) restrains
 Cu1, O11, C12, C13, C14, C15, C16, C17, N18, C19, C20, C21, C22, C23, C24,
 C25, O26, 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
4. Same fragment restrains
{Cu1, O11, C12, C13, C14, C15, C16, C17, N18, C19, C20, C21, C22, C23, C24,
C25, O26} sigma for 1-2: 0.01, 1-3: 0.02
as
{Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42, C43, C44,
C45, O46}
5. Others
 Fixed Sof: Cu1(0.5) O11(0.5) C12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
 C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) N18(0.5) C19(0.5) H19(0.5)
 C20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24(0.5) C25(0.5) O26(0.5) Cu2(0.5) O31(0.5) C32(0.5) C33(0.5) H33(0.5)
 C34(0.5) H34(0.5) C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) N38(0.5)
 C39(0.5) H39(0.5) C40(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5)
 H43(0.5) C44(0.5) H44(0.5) C45(0.5) O46(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C54(H54), 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)
6.b Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C40(C41,C42,C43,C44,C45)
;
_shelx_res_checksum              5037
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'