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

data_7711563
_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         'C22 H39 Cl3 O2 P2 Ti'
_chemical_formula_sum            'C22 H39 Cl3 O2 P2 Ti'
_chemical_formula_weight         551.76
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 99.419(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8749(2)
_cell_length_b                   10.5591(3)
_cell_length_c                   13.2857(3)
_cell_measurement_reflns_used    2381
_cell_measurement_temperature    173
_cell_measurement_theta_max      73
_cell_measurement_theta_min      5
_cell_volume                     1366.62(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_unetI/netI     0.077
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4812
_diffrn_reflns_theta_full        73.245
_diffrn_reflns_theta_max         73.245
_diffrn_reflns_theta_min         3.372
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.584
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 784 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.033(14)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     418
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.0396075
_refine_ls_shift/su_mean         0.0058062
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 0.09P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1360
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1360
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -8
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3251
_reflns_number_total             3568
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.13
_oxford_refine_ls_r_factor_ref   0.0553
_oxford_refine_ls_scale          2.754(18)
_oxford_reflns_number_all        3568
_oxford_structure_analysis_title 'T-2\FMC2102_autored.cif_od At 15: 8 on 17/10'
_cod_data_source_file            d2dt03291k4.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

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 21 '
_cod_database_code               7711563
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_hooft_y                  0.003(16)
_oxford_bijvoet_difference       -0.033(14)
_oxford_refined_flack_x          -0.028(13)