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_7700612
_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         'C31 H35 Cu N3 O2'
_chemical_formula_sum            'C31 H35 Cu N3 O2'
_chemical_formula_weight         545.16
_chemical_name_systematic        '[Cu(SB-1)](4-tBupy)2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-07
_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                 90.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3414(5)
_cell_length_b                   12.3024(3)
_cell_length_c                   24.5778(8)
_cell_measurement_reflns_used    18207
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5360
_cell_measurement_theta_min      1.9720
_cell_volume                     5545.7(3)
_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 0.999
_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    -89.00  22.00   1.00    5.00    --  -17.00 -72.00-180.00  111
  2  \w    -80.00  22.00   1.00    5.00    --  -17.00 -72.00 -17.00  102
  3  \w    -35.00  72.00   1.00    5.00    --  -17.00  72.00  81.00  107
  4  \w    -39.00   1.00   1.00    5.00    --  -17.00  -8.00 -50.00   40
  5  \w    -22.00  -7.00   1.00    5.00    --  -17.00  56.00 -50.00   15
  6  \w      3.00  18.00   1.00    5.00    --  -17.00 -56.00  16.00   15
  7  \w   -107.00  61.00   1.00    5.00    --  -17.00   8.00 -50.00  168
;
_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      -0.0364825000
_diffrn_orient_matrix_UB_12      0.0176806000
_diffrn_orient_matrix_UB_13      -0.0039448000
_diffrn_orient_matrix_UB_21      0.0081439000
_diffrn_orient_matrix_UB_22      0.0490919000
_diffrn_orient_matrix_UB_23      0.0138984000
_diffrn_orient_matrix_UB_31      0.0100134000
_diffrn_orient_matrix_UB_32      0.0245096000
_diffrn_orient_matrix_UB_33      -0.0249622000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70547
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.655
_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    0.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82202
_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    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_recrystallization_method
'Slow diffusion of water and isopropanol into solution of [Cu(SB-1)] in 4-tBupy'
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         12708
_refine_ls_number_restraints     1802
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0854P)^2^+5.0810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6240
_reflns_number_total             12708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           p1
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_database_code               7700612
_chemical_oxdiff_formula         Cu(C13H9N1O2)(C9H13N)
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. 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
Cu3 \\sim O51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim
N58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim
O66 \\sim Cu4 \\sim O71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim
C77 \\sim N78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim
C85 \\sim O86: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C21) = Uanis(C36)
Uanis(C23) = Uanis(C34)
Uanis(C52) = Uanis(C85)
Uanis(C74) = Uanis(C63)
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
 Cu3, O51, C52, C53, C54, C55, C56, C57, N58, C59, C60, C61, C62, C63, C64,
 C65, O66, Cu4, O71, C72, C73, C74, C75, C76, C77, N78, C79, C80, C81, C82, C83,
  C84, C85, O86
 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}
{Cu3, O51, C52, C53, C54, C55, C56, C57, N58, C59, C60, C61, C62, C63, C64,
C65, O66} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cu4, O71, C72, C73, C74, C75, C76, C77, N78, C79, C80, C81, C82, C83, C84,
C85, O86}
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)=Sof(Cu4)=Sof(O71)=Sof(C72)=Sof(C73)=Sof(H73)=Sof(C74)=
 Sof(H74)=Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(N78)=Sof(C79)=
 Sof(H79)=Sof(C80)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83)=
 Sof(C84)=Sof(H84)=Sof(C85)=Sof(O86)=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(Cu3)=Sof(O51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=
 Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(N58)=Sof(C59)=
 Sof(H59)=Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(O66)=FVAR(1)
6.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), C53(H53), C54(H54), C55(H55), C56(H56),
 C59(H59), C61(H61), C62(H62), C63(H63), C64(H64), C73(H73), C74(H74), C75(H75),
  C76(H76), C79(H79), C81(H81), C82(H82), C83(H83), C84(H84), C102(H102),
 C103(H103), C105(H105), C106(H106), C122(H122), C123(H123), C125(H125),
 C126(H126), C142(H142), C143(H143), C145(H145), C146(H146), C162(H162),
 C163(H163), C165(H165), C166(H166)
6.b Idealised Me refined as rotating group:
 C108(H10A,H10B,H10C), C109(H10D,H10E,H10F), C110(H11A,H11B,H11C), C128(H12A,
 H12B,H12C), C129(H12D,H12E,H12F), C130(H13A,H13B,H13C), C148(H14A,H14B,H14C),
 C149(H14D,H14E,H14F), C150(H15A,H15B,H15C), C168(H16A,H16B,H16C), C169(H16D,
 H16E,H16F), C170(H17A,H17B,H17C)
;
_shelx_res_checksum              78190
_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 2.338
_oxdiff_exptl_absorpt_empirical_full_min 0.470