Synthesis of compounds with C-P-P and C[double bond, length as m-dash]P-P bond systems based on the phospha-Wittig reaction.
Ziółkowska, Aleksandra; Szynkiewicz, Natalia; Pikies, Jerzy; Ponikiewski, Łukasz; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13635–13646; doi:10.1039/d0dt02728f

data_7705362
_publ_section_title
;
 Synthesis of compounds with C-P-P and C[double bond, length as m-dash]P-P
 bond systems based on the phospha-Wittig reaction.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13635
_journal_page_last               13646
_journal_paper_doi               10.1039/d0dt02728f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H64 Cl1 N2 O2 Ti1'
_chemical_formula_sum            'C43 H64 Cl N2 O2 Ti'
_chemical_formula_weight         724.31
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2020-09-01T12:23:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-09-02 deposited with the CCDC.	2020-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.089(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6443(16)
_cell_length_b                   18.6688(7)
_cell_length_c                   19.2429(10)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.83
_cell_measurement_wavelength     0.71073
_cell_volume                     8027.0(8)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017) 
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_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 0.99
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      ' 183 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27717
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.217
_diffrn_reflns_theta_min         2.24
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.62
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     464
_refine_ls_number_reflns         10746
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+5.1550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.214
_reflns_Friedel_coverage         0
_reflns_number_gt                6015
_reflns_number_total             10746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02728f2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7705360--7705366.cif.'
_cod_original_cell_volume        8026.9(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7705362
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.96