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_7700182
_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         'C25 H24 Cl N6 P Pd'
_chemical_formula_sum            'C25 H24 Cl N6 P Pd'
_chemical_formula_weight         581.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0270(18)
_cell_length_b                   15.942(3)
_cell_length_c                   17.225(3)
_cell_measurement_reflns_used    12715
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      1.74
_cell_volume                     2478.8(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0552
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9518
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         1.741
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.7707
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 1779 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_coef       0.0058(10)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5395
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0774P)^2^+4.5303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4616
_reflns_number_total             5395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02057h2.cif
_cod_data_source_block           hw_b
_cod_depositor_comments
'Adding full bibliography for 7700175--7700185.cif.'
_cod_original_cell_volume        2478.8(9)
_cod_database_code               7700182
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5) H2AA(0.5) H2AB(0.5)
 H2BC(0.5) H2BD(0.5) C3(0.5) H3(0.5) C5(0.5) H5(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C2(H2AA,H2AB), C2(H2BC,H2BD)
4.c Aromatic/amide H refined with riding coordinates:
 C205(H205), C103(H103), C20(H20), C102(H102), C32(H32), C10(H10), C22(H22),
 C201(H201), C31(H31), C21(H21), C105(H105), C11(H11), C101(H101), C30(H30),
 C202(H202), C203(H203), C12(H12), C104(H104), C204(H204)
;
_shelx_res_checksum              67419
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in perfluoroether oil'
_olex2_submission_original_sample_id LS2
_olex2_submission_special_instructions 'No special instructions were received'