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_7700609
_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
_chemical_name_systematic        '[Cu(SB-1)](4-dmap)2'
_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     iterative
_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                 94.861(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   35.0007(9)
_cell_length_b                   12.6364(4)
_cell_length_c                   16.9160(4)
_cell_measurement_reflns_used    18422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4090
_cell_measurement_theta_min      2.0850
_cell_volume                     7454.7(4)
_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
;
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 0.993
_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    -55.00  74.00   1.00   10.00    --  -16.00  72.00  30.00  129
  2  \w   -103.00  19.00   1.00   10.00    --  -16.00 -54.00 -60.00  122
  3  \w    -85.00 -35.00   1.00   10.00    --  -16.00 -72.00  90.00   50
  4  \w     14.00  35.00   1.00   10.00    --  -16.00  72.00   0.00   21
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0201888000
_diffrn_orient_matrix_UB_12      -0.0052603000
_diffrn_orient_matrix_UB_13      -0.0067496000
_diffrn_orient_matrix_UB_21      0.0019938000
_diffrn_orient_matrix_UB_22      -0.0146413000
_diffrn_orient_matrix_UB_23      -0.0399299000
_diffrn_orient_matrix_UB_31      0.0013972000
_diffrn_orient_matrix_UB_32      -0.0539219000
_diffrn_orient_matrix_UB_33      0.0115004000
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.714
_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    0.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             3252
_exptl_crystal_recrystallization_method
'Slow diffusion of water into DMSO solution'
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         16992
_refine_ls_number_restraints     2311
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0544P)^2^+9.7485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11750
_reflns_number_total             16992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01527b2.cif
_cod_data_source_block           2015tdk096_s1
_cod_depositor_comments
'Adding full bibliography for 7700601--7700615.cif.'
_cod_database_code               7700609
_chemical_oxdiff_formula         (CuC13H9NO2)(C7H10N2)2
_reflns_odcompleteness_completeness 99.34
_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. Uiso/Uaniso restraints and constraints
Cu11 \\sim O111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim
C117 \\sim N118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim
C124 \\sim C125 \\sim O126 \\sim Cu12 \\sim O131 \\sim C132 \\sim C133 \\sim
C134 \\sim C135 \\sim C136 \\sim C137 \\sim N138 \\sim C139 \\sim C140 \\sim
C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim O146: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Cu21 \\sim O211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim
C217 \\sim N218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223 \\sim
C224 \\sim C225 \\sim O226 \\sim Cu22 \\sim O231 \\sim C232 \\sim C233 \\sim
C234 \\sim C235 \\sim C236 \\sim C237 \\sim N238 \\sim C239 \\sim C240 \\sim
C241 \\sim C242 \\sim C243 \\sim C244 \\sim C245 \\sim O246: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Cu31 \\sim O311 \\sim C312 \\sim C313 \\sim C314 \\sim C315 \\sim C316 \\sim
C317 \\sim N318 \\sim C319 \\sim C320 \\sim C321 \\sim C322 \\sim C323 \\sim
C324 \\sim C325 \\sim O326 \\sim Cu32 \\sim O331 \\sim C332 \\sim C333 \\sim
C334 \\sim C335 \\sim C336 \\sim C337 \\sim N338 \\sim C339 \\sim C340 \\sim
C341 \\sim C342 \\sim C343 \\sim C344 \\sim C345 \\sim O346: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Cu22) = Uanis(Cu21)
3. Rigid body (RIGU) restrains
 Cu11, O111, C112, C113, C114, C115, C116, C117, N118, C119, C120, C121, C122,
 C123, C124, C125, O126, Cu12, O131, C132, C133, C134, C135, C136, C137, N138,
 C139, C140, C141, C142, C143, C144, C145, O146
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu21, O211, C212, C213, C214, C215, C216, C217, N218, C219, C220, C221, C222,
 C223, C224, C225, O226, Cu22, O231, C232, C233, C234, C235, C236, C237, N238,
 C239, C240, C241, C242, C243, C244, C245, O246
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu31, O311, C312, C313, C314, C315, C316, C317, N318, C319, C320, C321, C322,
 C323, C324, C325, O326, Cu32, O331, C332, C333, C334, C335, C336, C337, N338,
 C339, C340, C341, C342, C343, C344, C345, O346
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Cu31, O311, C312, C313, C314, C315, C316, C317, N318, C319, C320, C321, C322,
C323, C324, C325, O326} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cu32, O331, C332, C333, C334, C335, C336, C337, N338, C339, C340, C341, C342,
C343, C344, C345, O346}
{Cu11, O111, C112, C113, C114, C115, C116, C117, N118, C119, C120, C121, C122,
C123, C124, C125, O126} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cu12, O131, C132, C133, C134, C135, C136, C137, N138, C139, C140, C141, C142,
C143, C144, C145, O146}
{Cu21, O211, C212, C213, C214, C215, C216, C217, N218, C219, C220, C221, C222,
C223, C224, C225, O226} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cu22, O231, C232, C233, C234, C235, C236, C237, N238, C239, C240, C241, C242,
C243, C244, C245, O246}
5. Others
 Sof(Cu12)=Sof(O131)=Sof(C132)=Sof(C133)=Sof(H133)=Sof(C134)=Sof(H134)=
 Sof(C135)=Sof(H135)=Sof(C136)=Sof(H136)=Sof(C137)=Sof(N138)=Sof(C139)=
 Sof(H139)=Sof(C140)=Sof(C141)=Sof(H141)=Sof(C142)=Sof(H142)=Sof(C143)=
 Sof(H143)=Sof(C144)=Sof(H144)=Sof(C145)=Sof(O146)=1-FVAR(1)
 Sof(Cu11)=Sof(O111)=Sof(C112)=Sof(C113)=Sof(H113)=Sof(C114)=Sof(H114)=
 Sof(C115)=Sof(H115)=Sof(C116)=Sof(H116)=Sof(C117)=Sof(N118)=Sof(C119)=
 Sof(H119)=Sof(C120)=Sof(C121)=Sof(H121)=Sof(C122)=Sof(H122)=Sof(C123)=
 Sof(H123)=Sof(C124)=Sof(H124)=Sof(C125)=Sof(O126)=FVAR(1)
 Sof(Cu22)=Sof(O231)=Sof(C232)=Sof(C233)=Sof(H233)=Sof(C234)=Sof(H234)=
 Sof(C235)=Sof(H235)=Sof(C236)=Sof(H236)=Sof(C237)=Sof(N238)=Sof(C239)=
 Sof(H239)=Sof(C240)=Sof(C241)=Sof(H241)=Sof(C242)=Sof(H242)=Sof(C243)=
 Sof(H243)=Sof(C244)=Sof(H244)=Sof(C245)=Sof(O246)=1-FVAR(2)
 Sof(Cu21)=Sof(O211)=Sof(C212)=Sof(C213)=Sof(H213)=Sof(C214)=Sof(H214)=
 Sof(C215)=Sof(H215)=Sof(C216)=Sof(H216)=Sof(C217)=Sof(N218)=Sof(C219)=
 Sof(H219)=Sof(C220)=Sof(C221)=Sof(H221)=Sof(C222)=Sof(H222)=Sof(C223)=
 Sof(H223)=Sof(C224)=Sof(H224)=Sof(C225)=Sof(O226)=FVAR(2)
 Sof(Cu32)=Sof(O331)=Sof(C332)=Sof(C333)=Sof(H333)=Sof(C334)=Sof(H334)=
 Sof(C335)=Sof(H335)=Sof(C336)=Sof(H336)=Sof(C337)=Sof(N338)=Sof(C339)=
 Sof(H339)=Sof(C340)=Sof(C341)=Sof(H341)=Sof(C342)=Sof(H342)=Sof(C343)=
 Sof(H343)=Sof(C344)=Sof(H344)=Sof(C345)=Sof(O346)=1-FVAR(3)
 Sof(Cu31)=Sof(O311)=Sof(C312)=Sof(C313)=Sof(H313)=Sof(C314)=Sof(H314)=
 Sof(C315)=Sof(H315)=Sof(C316)=Sof(H316)=Sof(C317)=Sof(N318)=Sof(C319)=
 Sof(H319)=Sof(C320)=Sof(C321)=Sof(H321)=Sof(C322)=Sof(H322)=Sof(C323)=
 Sof(H323)=Sof(C324)=Sof(H324)=Sof(C325)=Sof(O326)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C313(H313), C314(H314), C315(H315), C316(H316), C319(H319), C321(H321),
 C322(H322), C323(H323), C324(H324), C333(H333), C334(H334), C335(H335),
 C336(H336), C339(H339), C341(H341), C342(H342), C343(H343), C344(H344),
 C352(H352), C353(H353), C355(H355), C356(H356), C362(H362), C363(H363),
 C365(H365), C366(H366), C113(H113), C114(H114), C115(H115), C116(H116),
 C119(H119), C121(H121), C122(H122), C123(H123), C124(H124), C133(H133),
 C134(H134), C135(H135), C136(H136), C139(H139), C141(H141), C142(H142),
 C143(H143), C144(H144), C152(H152), C153(H153), C155(H155), C156(H156),
 C162(H162), C163(H163), C165(H165), C166(H166), C213(H213), C214(H214),
 C215(H215), C216(H216), C219(H219), C221(H221), C222(H222), C223(H223),
 C224(H224), C233(H233), C234(H234), C235(H235), C236(H236), C239(H239),
 C241(H241), C242(H242), C243(H243), C244(H244), C252(H252), C253(H253),
 C255(H255), C256(H256), C262(H262), C263(H263), C265(H265), C266(H266)
6.b Idealised Me refined as rotating group:
 C358(H35A,H35B,H35C), C359(H35D,H35E,H35F), C368(H36A,H36B,H36C), C369(H36D,
 H36E,H36F), C158(H15A,H15B,H15C), C159(H15D,H15E,H15F), C168(H16A,H16B,H16C),
 C169(H16D,H16E,H16F), C258(H25A,H25B,H25C), C259(H25D,H25E,H25F), C268(H26A,
 H26B,H26C), C269(H26D,H26E,H26F)
;
_shelx_res_checksum              33282
_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 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.768