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_7700175
_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 N6 P'
_chemical_formula_sum            'C22 H19 N6 P'
_chemical_formula_weight         398.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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            12
_cell_length_a                   17.416(4)
_cell_length_b                   8.4390(17)
_cell_length_c                   40.806(8)
_cell_measurement_reflns_used    63347
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      1.50
_cell_volume                     5997(2)
_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  0.0935
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            80621
_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         25.999
_diffrn_reflns_theta_min         1.497
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2496
_exptl_crystal_recrystallization_method
'The material was recrystallised from toluene by slow evaporation'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.379
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 4453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.0058(7)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         11783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0884P)^2^+3.0083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1631
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10540
_reflns_number_total             11783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02057h2.cif
_cod_data_source_block           hw_a
_cod_depositor_comments
'Adding full bibliography for 7700175--7700185.cif.'
_cod_database_code               7700175
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(13)
 0.09(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C404(H404), C22(H22), C301(H301), C61(H61), C60(H60), C405(H405), C80(H80),
 C50(H50), C20(H20), C40(H40), C52(H52), C30(H30), C62(H62), C203(H203),
 C32(H32), C31(H31), C603(H603), C602(H602), C101(H101), C303(H303), C21(H21),
 C82(H82), C201(H201), C10(H10), C92(H92), C42(H42), C102(H102), C41(H41),
 C12(H12), C70(H70), C302(H302), C601(H601), C9(H9), C11(H11), C304(H304),
 C103(H103), C72(H72), C604(H604), C51(H51), C305(H305), C81(H81), C605(H605),
 C17(H17), C18(H18), C71(H71), C90(H90), C19(H19), C401(H401), C505(H505),
 C403(H403), C1F(H1F), C402(H402), C91(H91), C501(H501), C502(H502), C504(H504),
  C503(H503)
;
_shelx_res_checksum              53460
_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 HW71
_olex2_submission_special_instructions 'No special instructions were received'