Pd(II), Ni(II), and Cu(II) complexes of α,α'-ditolylmethanone dipyrroethene.
Pushpanandan, Poornenth; Behera, Kanhu Charan; Ravikanth, Mangalampalli; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00476g

data_7712982
_publ_section_title
;
 Pd(II), Ni(II), and Cu(II) complexes of &#x3b1;,&#x3b1;'-ditolylmethanone
 dipyrroethene.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00476g
_journal_year                    2023
_chemical_formula_moiety         'C40 H32 N2 O2 Pd'
_chemical_formula_sum            'C40 H32 N2 O2 Pd'
_chemical_formula_weight         679.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-11-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2023-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                81.174(4)
_cell_angle_beta                 65.549(4)
_cell_angle_gamma                88.541(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4482(4)
_cell_length_b                   11.8734(5)
_cell_length_c                   12.9557(5)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.5860
_cell_measurement_theta_min      1.7340
_cell_volume                     1582.72(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -10.27 349.73   1.00   10.00  72.70 -18.16  31.50    --   360
  2  \w    -76.15   6.85   1.00   10.00    --  -18.16  89.85-137.67   83
  3  \w    -76.15   6.85   1.00   10.00    --  -18.16  89.85  69.33   83
  4  \w   -122.88  23.12   1.00   10.00    --  -18.16 -59.25-135.92  146
  5  \w    -76.15   6.85   1.00   10.00    --  -18.16  89.85 -32.67   83
  6  \w   -122.88  23.12   1.00   10.00    --  -18.16 -59.25  71.08  146
  7  \f    -71.73  10.27   1.00   10.00  31.10 -18.16 -31.50    --    82
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0946
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27860
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.737
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.425
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0438
_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^)+0.8791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4746
_reflns_number_total             5578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00476g2.cif
_cod_data_source_block           mr_prp_pd2_autored
_cod_database_code               7712982
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.969
_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.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00A), C00D(H00D), C00G(H00G), C00O(H00O), C00P(H00P),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C010(H010), C012(H012), C013(H013), C014(H014), C015(H015)
2.b Idealised Me refined as rotating group:
 C016(H01A,H01B,H01C), C017(H01D,H01E,H01F), C018(H01G,H01H,H01I), C019(H01J,
 H01K,H01L)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15657
_shelx_hkl_checksum              38097
_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
;