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

data_7711564
_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_formula_moiety         'C28 H44 Br1 O2 P2 Ti1'
_chemical_formula_sum            'C28 H44 Br O2 P2 Ti'
_chemical_formula_weight         602.41
_chemical_melting_point          ?
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.7926(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4564(2)
_cell_length_b                   12.7270(2)
_cell_length_c                   15.5888(2)
_cell_measurement_reflns_used    4024
_cell_measurement_temperature    173
_cell_measurement_theta_max      73.07
_cell_measurement_theta_min      3.76
_cell_volume                     3038.21(7)
_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_max 0.948
_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  0.042
_diffrn_reflns_av_unetI/netI     0.077
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10033
_diffrn_reflns_theta_full        73.525
_diffrn_reflns_theta_max         73.525
_diffrn_reflns_theta_min         3.779
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.084
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     799
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.0046890
_refine_ls_shift/su_mean         0.0006436
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method = Chebychev polynomial, (Carruthers & Watkin, 1979) 
 W = 1.0/[A[0]*T[0]'(X)+A[1]*T[1]'(X) ... +A[NP-1]*T[NP-1]'(X)] 
 146. 177. 44.8 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1124
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.1124
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4303
_reflns_number_total             5799
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.38
_oxford_refine_ls_r_factor_ref   0.0629
_oxford_refine_ls_scale          1.3013(19)
_oxford_reflns_number_all        5799
_cod_data_source_file            d2dt03291k4.cif
_cod_data_source_block           6B
_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/n '
_cod_original_formula_sum        'C28 H44 Br1 O2 P2 Ti1'
_cod_database_code               7711564
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0629
_oxford_refine_ls_wr_factor_all  0.1124