Phosphanylphosphaalkenes as precursors for metallaphosphaalkene complexes.
Ziółkowska, Aleksandra; Kruczyński, Tomasz; Gudat, Dietrich; Ponikiewski, Łukasz; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19107–19111; doi:10.1039/d4dt03012e

data_7717490
_publ_section_title
;
 Phosphanylphosphaalkenes as precursors for metallaphosphaalkene
 complexes.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19107
_journal_page_last               19111
_journal_paper_doi               10.1039/d4dt03012e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C45 H46 Cl3 P Ru2'
_chemical_formula_sum            'C45 H46 Cl3 P Ru2'
_chemical_formula_weight         926.28
_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
_audit_creation_date             2024-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                74.161(2)
_cell_angle_beta                 78.653(2)
_cell_angle_gamma                87.765(2)
_cell_formula_units_Z            4
_cell_length_a                   16.3325(5)
_cell_length_b                   16.6265(5)
_cell_length_c                   16.9118(5)
_cell_measurement_reflns_used    111251
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      1.97
_cell_volume                     4331.2(2)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.88, Darmstadt 2019
;
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      '409 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.636
_diffrn_reflns_theta_min         1.968
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.1623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         23279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+8.8334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1327
_reflns_d_resolution_high        0.719
_reflns_d_resolution_low         10.347
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                18255
_reflns_number_total             23279
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d4dt03012e2.cif
_cod_data_source_block           za13_2024
_cod_depositor_comments
'Adding full bibliography for 7717484--7717490.cif.'
_cod_database_code               7717490
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.871
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C33(H33), C43(H43), C78(H78), C88(H88)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C37(H37),
 C38(H38), C40(H40), C41(H41), C48(H48), C49(H49), C51(H51), C52(H52), C54(H54),
  C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C63(H63),
 C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73),
  C75(H75), C76(H76), C82(H82), C83(H83), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C),
 C90(H90A,H90B,H90C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55735
_shelx_hkl_checksum              62397
_shelx_fab_checksum              57075
_olex2_submission_special_instructions 'No special instructions were received'