Direct synthesis of doubly deprotonated, dearomatised lutidine PNP Cr and Zr pincer complexes based on isolated K and Li ligand transfer reagents.
Simler, Thomas; Frison, Gilles; Braunstein, Pierre; Danopoulos, Andreas A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2800–2804; doi:10.1039/c6dt00144k

data_7038050
_publ_section_title
;
 Direct synthesis of doubly deprotonated, dearomatised lutidine PNP Cr and
 Zr pincer complexes based on isolated K and Li ligand transfer reagents.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2800
_journal_page_last               2804
_journal_paper_doi               10.1039/c6dt00144k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C46 H82 Cl2 Cr3 N2 P4'
_chemical_formula_sum            'C46 H82 Cl2 Cr3 N2 P4'
_chemical_formula_weight         1013.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-25 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0266(14)
_cell_length_b                   18.1629(15)
_cell_length_c                   19.1642(15)
_cell_measurement_reflns_used    4430
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.44
_cell_volume                     5926.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1268
_diffrn_reflns_av_unetI/netI     0.1927
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.011
_diffrn_reflns_theta_min         1.545
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
 The residual electron density was assigned to a molecule of the
 pentane solvent [142/4 = 36 e per asymmetric unit; one molecule of
 C5H12 would give 42e].
;
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 2168 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         14278
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.829
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.995
_reflns_number_gt                7075
_reflns_number_total             14278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00144k2.cif
_cod_data_source_block           pbts150804
_cod_depositor_comments
'Adding full bibliography for 7038049--7038051.cif.'
_cod_database_code               7038050
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.894
_shelxl_version_number           2013-4
_shelx_res_checksum              47470