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_7700614
_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         'C27 H29 Cu N5 O2'
_chemical_formula_sum            'C27 H29 Cu N5 O2'
_chemical_formula_weight         519.09
_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
_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                 110.895(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2309(5)
_cell_length_b                   19.1471(6)
_cell_length_c                   11.1735(4)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4830
_cell_measurement_theta_min      2.2700
_cell_volume                     2444.60(17)
_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    '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 0.998
_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  44.00   1.00    4.00    --  -17.00 -18.00  30.00  151
  2  \w    -53.00  22.00   1.00    4.00    --  -17.00 -72.00 120.00   75
  3  \w    -29.00  73.00   1.00    4.00    --  -17.00  72.00  30.00  102
  4  \w    -72.00 -57.00   1.00    4.00    --  -17.00 -18.00-180.00   15
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  Ros
_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      -0.0454317000
_diffrn_orient_matrix_UB_12      -0.0244549000
_diffrn_orient_matrix_UB_13      -0.0072149000
_diffrn_orient_matrix_UB_21      -0.0423490000
_diffrn_orient_matrix_UB_22      0.0263186000
_diffrn_orient_matrix_UB_23      -0.0277377000
_diffrn_orient_matrix_UB_31      -0.0000848000
_diffrn_orient_matrix_UB_32      -0.0089715000
_diffrn_orient_matrix_UB_33      -0.0616160000
_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  0.0268
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19122
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.374
_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    0.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92796
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_recrystallization_method
'Slow diffusion of water into DMSO solution'
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0431P)^2^+1.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4783
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           2015tdk108
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_original_cell_volume        2444.59(17)
_cod_database_code               7700614
_chemical_oxdiff_formula         Cu1(C13H9N1O2)(C7H10N2)
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 Cu1-Cu2
 -0.6 with sigma of 0.01
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: 0.02, 1-3: 0.04
as
{Cu2, O31, C32, C33, C34, C35, C36, C37, N38, C39, C40, C41, C42, C43, C44,
C45, O46}
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C65(H65), C63(H63), C52(H52), C56(H56), C53(H53), C66(H66), C55(H55),
 C62(H62), 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 Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C59(H59A,H59B,
 H59C)
;
_shelx_res_checksum              19555
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method Mitegen
_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 1.702
_oxdiff_exptl_absorpt_empirical_full_min 0.531