Synthesis and reactivity of titanium ‘POCOP’ pincer complexes
Webster, Leah; Krämer, Tobias; Chadwick, F. Mark; Dalton Transactions  (2022) –; doi:10.1039/D2DT03291K

data_7711560
_publ_section_title
;
 Synthesis and reactivity of titanium &#x2018;POCOP&#x2019; pincer
 complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03291K
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H78 Li2 O4 P4'
_chemical_formula_sum            'C44 H78 Li2 O4 P4'
_chemical_formula_weight         808.88
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9510(7)
_cell_length_b                   14.8413(5)
_cell_length_c                   15.1618(4)
_cell_measurement_reflns_used    1789
_cell_measurement_temperature    173
_cell_measurement_theta_max      72
_cell_measurement_theta_min      4
_cell_volume                     4939.4(3)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_unetI/netI     0.115
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10545
_diffrn_reflns_theta_full        73.278
_diffrn_reflns_theta_max         73.278
_diffrn_reflns_theta_min         3.595
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.42
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1943 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.00(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7239
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.0002180
_refine_ls_shift/su_mean         0.0000138
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 5.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1615
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1615
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -18
_reflns_number_gt                5360
_reflns_number_total             7239
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      0.89
_oxford_refine_ls_r_factor_ref   0.0930
_oxford_refine_ls_scale          1.099(5)
_oxford_reflns_number_all        7239
_cod_data_source_file            d2dt03291k4.cif
_cod_data_source_block           LitBuPOCOP
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_database_code               7711560
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_hooft_y                  -0.04(4)
_oxford_bijvoet_difference       -0.00(4)