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

data_7711562
_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         'C36 H62 Cl6 O4 P4 Ti2'
_chemical_formula_sum            'C36 H62 Cl6 O4 P4 Ti2'
_chemical_formula_weight         991.30
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.440(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9525(3)
_cell_length_b                   13.0318(2)
_cell_length_c                   15.1944(4)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    173
_cell_measurement_theta_max      73
_cell_measurement_theta_min      4
_cell_volume                     2319.70(9)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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 0.977
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.058
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13979
_diffrn_reflns_theta_full        68.271
_diffrn_reflns_theta_max         73.409
_diffrn_reflns_theta_min         3.773
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.695
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.5275
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.0004878
_refine_ls_shift/su_mean         0.0000955
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.213E+04 0.354E+04 0.220E+04 931. 214. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1729
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1729
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3840
_reflns_number_total             4544
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0656
_oxford_refine_ls_scale          3.46(6)
_oxford_reflns_number_all        4544
_cod_data_source_file            d2dt03291k4.cif
_cod_data_source_block           4
_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 21/c '
_cod_database_code               7711562
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)