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_7712983
_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 Ni O2'
_chemical_formula_sum            'C40 H32 N2 Ni O2'
_chemical_formula_weight         631.38
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                96.813(4)
_cell_angle_beta                 106.561(4)
_cell_angle_gamma                96.781(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8300(5)
_cell_length_b                   11.2853(6)
_cell_length_c                   14.8021(6)
_cell_measurement_reflns_used    7457
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      22.8330
_cell_measurement_theta_min      1.8100
_cell_volume                     1542.80(14)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_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  \f   -349.73  10.27   1.00    3.00   9.41 -12.98 -31.50    --   360
  2  \w    -65.46  -0.46   1.00    3.00    --  -15.96  94.56 145.16   65
  3  \w    -68.96   0.04   1.00    3.00    --  -19.47  94.56 -34.84   69
  4  \w   -108.63  15.37   1.00    3.00    --  -12.98 -59.25 -33.92  124
  5  \w   -108.63  15.37   1.00    3.00    --  -12.98 -59.25 173.08  124
  6  \w    -65.46  -0.46   1.00    3.00    --  -15.96  94.56   1.16   65
  7  \f   -339.92  20.08   1.00    3.00  16.12 -12.98 -59.25    --   360
  8  \w    -65.46  -0.46   1.00    3.00    --  -15.96  94.56  73.16   65
  9  \w   -108.63  15.37   1.00    3.00    --  -12.98 -59.25  20.08  124
 10  \w    -55.98   0.02   1.00    3.00    --   -6.49  94.56 -34.84   56
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120243000
_diffrn_orient_matrix_UB_12      -0.0596660000
_diffrn_orient_matrix_UB_13      -0.0252165000
_diffrn_orient_matrix_UB_21      -0.0468643000
_diffrn_orient_matrix_UB_22      0.0178495000
_diffrn_orient_matrix_UB_23      -0.0403485000
_diffrn_orient_matrix_UB_31      0.0589434000
_diffrn_orient_matrix_UB_32      0.0152587000
_diffrn_orient_matrix_UB_33      -0.0173516000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1732
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56131
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17275
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.0821
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0851P)^2^+0.3147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4077
_reflns_number_total             5438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00476g2.cif
_cod_data_source_block           mr_prp_ni_di_autored
_cod_original_cell_volume        1542.80(13)
_cod_database_code               7712983
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 79.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     35.60
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00U(0.044) H00H(0.044) H00B(0.041) H00M(0.04) H00T(0.045)
 H00W(0.049) H00Y(0.049) H013(0.046) H01D(0.069) H01E(0.069) H01F(0.069)
 H00I(0.041) H00O(0.044) H011(0.044) H00Q(0.043) H01A(0.065) H01B(0.065)
 H01C(0.065) H012(0.05) H016(0.057) H010(0.045) H00P(0.04) H01J(0.09)
 H01K(0.09) H01L(0.09) H00F(0.04) H00X(0.046) H00R(0.042) H008(0.042)
 H01G(0.083) H01H(0.083) H01I(0.083)
 Fixed X: H00U(0.581685) H00H(0.495664) H00B(-0.067608) H00M(-0.130103)
 H00T(0.414301) H00W(0.532605) H00Y(0.734284) H013(0.613419) H01D(0.68299)
 H01E(0.824639) H01F(0.707638) H00I(0.493987) H00O(0.59373) H011(0.273762)
 H00Q(0.172931) H01A(0.607886) H01B(0.452851) H01C(0.502351) H012(0.229906)
 H016(0.111658) H010(-0.22253) H00P(-0.103762) H01J(-0.174156) H01K(-0.079436)
 H01L(-0.229928) H00F(-0.21696) H00X(-0.311624) H00R(0.056568) H008(0.149616)
 H01G(-0.116047) H01H(-0.264857) H01I(-0.241695)
 Fixed Y: H00U(0.418343) H00H(0.574807) H00B(0.839026) H00M(0.786653)
 H00T(0.269728) H00W(0.114342) H00Y(0.124432) H013(0.277306) H01D(-0.074285)
 H01E(0.021405) H01F(-0.013652) H00I(0.839578) H00O(0.905367) H011(0.688771)
 H00Q(0.622924) H01A(0.834403) H01B(0.800251) H01C(0.932813) H012(0.957123)
 H016(1.084423) H010(0.815779) H00P(0.686235) H01J(1.10871) H01K(1.085001)
 H01L(0.999927) H00F(0.651499) H00X(0.668931) H00R(0.596654) H008(0.57161)
 H01G(0.682575) H01H(0.706219) H01I(0.571431)
 Fixed Z: H00U(0.756437) H00H(0.848335) H00B(0.583178) H00M(0.406283)
 H00T(0.381521) H00W(0.343868) H00Y(0.623384) H013(0.661769) H01D(0.474382)
 H01E(0.489946) H01F(0.386726) H00I(0.846573) H00O(1.009592) H011(1.056916)
 H00Q(0.894615) H01A(1.176922) H01B(1.190266) H01C(1.171196) H012(0.782792)
 H016(0.858733) H010(0.802827) H00P(0.729869) H01J(0.848265) H01K(0.949992)
 H01L(0.895544) H00F(0.263134) H00X(0.10311) H00R(0.055315) H008(0.213179)
 H01G(-0.063076) H01H(-0.04604) H01I(-0.077922)
;
_shelx_res_checksum              51978
_shelx_hkl_checksum              16417
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.542
_oxdiff_exptl_absorpt_empirical_full_min 0.455