Phosphine-functionalised tris(pyrazolyl)methane ligands and their mono- and heterobimetallic complexes.
Wagner, Hanna E.; Hohnstein, Silvia; Schußmann, Max G; Steppe, Lukas A.; Breher, Frank; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15397–15407; doi:10.1039/c9dt02057h

data_7700181
_publ_section_title
;
 Phosphine-functionalised tris(pyrazolyl)methane ligands and their mono-
 and heterobimetallic complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15397
_journal_page_last               15407
_journal_paper_doi               10.1039/c9dt02057h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H19 Cl2 N6 P Pd'
_chemical_formula_sum            'C22 H19 Cl2 N6 P Pd'
_chemical_formula_weight         575.70
_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     dual
_audit_creation_date             2019-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.818(3)
_cell_length_b                   9.2710(19)
_cell_length_c                   16.998(3)
_cell_measurement_reflns_used    11884
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      1.40
_cell_volume                     2292.6(8)
_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      200
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15955
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.174
_diffrn_reflns_theta_min         1.400
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.8475
_exptl_absorpt_correction_T_min  0.7392
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Stoe & Cie, X-RED, version 1.28b: Program for data reduction and absorptioncorrection, Stoe &CieGmbH, Darmatadt, Germany, 2005.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.3641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5251
_reflns_number_total             6154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02057h2.cif
_cod_data_source_block           hw_a_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7700175--7700185.cif.'
_cod_original_cell_volume        2292.7(8)
_cod_database_code               7700181
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.659
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C205(H205), C101(H101), C105(H105), C201(H201), C102(H102), C30(H30),
 C10(H10), C12(H12), C11(H11), C204(H204), C104(H104), C103(H103), C202(H202),
 C203(H203), C31(H31), C20(H20), C32(H32), C22(H22), C21(H21)
;
_shelx_res_checksum              19324
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id MGS17
_olex2_submission_special_instructions 'No special instructions were received'