Synthesis, Structure, and Properties of Palladium(II) Complex of α-Formyl Pyrrolyl Dipyrromethene
Panchavarnam, Sabari; Sengupta, Rima; Ravikanth, Mangalampalli; Dalton Transactions  (2022) –; doi:10.1039/D2DT00166G

data_7709708
_publ_section_title
;
 Synthesis, Structure, and Properties of Palladium(II) Complex of
 \a-Formyl Pyrrolyl Dipyrromethene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00166G
_journal_year                    2022
_chemical_formula_moiety         'C21 H16 B F2 N3 O'
_chemical_formula_sum            'C21 H16 B F2 N3 O'
_chemical_formula_weight         375.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     direct
_audit_creation_date             2021-12-13
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-12-13 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1997(8)
_cell_length_b                   15.3185(11)
_cell_length_c                   22.490(2)
_cell_measurement_reflns_used    877
_cell_measurement_temperature    105(7)
_cell_measurement_theta_max      18.6520
_cell_measurement_theta_min      2.6570
_cell_volume                     3513.9(5)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      105.15
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_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     75.79 204.29   0.50    5.00  15.81  -9.84 -59.25    --   257
  2  \w   -100.81  15.69   0.50    5.00    --   -9.84 -59.25  20.08  233
;
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2034
_diffrn_reflns_av_unetI/netI     0.2269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33811
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81024
_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            'metallic dark pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.4183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552.8330
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.4076
_refine_diff_density_min         -0.4693
_refine_diff_density_rms         0.1107
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.6593
_refine_ls_goodness_of_fit_ref   1.0400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0400
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+1.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                1999
_reflns_number_total             3093
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt00166g2.cif
_cod_data_source_block           mr_ps_bdy_cho_autored
_cod_database_code               7709708
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C20(H20), C14(H14), C12(H12), C3(H3), C8(H8), C4(H4), C7(H7),
 C19(H19), C17(H17), C16(H16), C1(H1a), C13(H13)
2.b Idealised Me refined as rotating group:
 C21(H21b,H21c,H21a)
;
_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
;