Single step, high yield synthesis of para-hydroxy functionalized POCOP ligands and their Ni(ii) pincer derivatives
García-Eleno, Marco A.; Padilla-Mata, Esteban; Estudiante-Negrete, Fabiola; Pichal-Cerda, Francisco; Hernández-Ortega, Simón; Toscano, Rubén A.; Morales-Morales, David; New J. Chem. 39 (2015) 3361–; doi:10.1039/C5NJ00052A

data_7054732
_publ_section_title
;
 Single step, high yield synthesis of para-hydroxy functionalized POCOP
 ligands and their Ni(ii) pincer derivatives
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              3361
_journal_paper_doi               10.1039/C5NJ00052A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C22 H39 Cl Ni O3 P2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H40 Cl2 Ni O3 P2'
_chemical_formula_weight         550.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-02-20 deposited with the CCDC.
2015-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.917(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1590(11)
_cell_length_b                   20.230(2)
_cell_length_c                   13.9587(15)
_cell_measurement_reflns_used    6248
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.26
_cell_volume                     2796.2(5)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 7.34A (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.377
_diffrn_reflns_theta_min         1.804
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_correction_T_min  0.7769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5123
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0628P)^2^+0.5704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3903
_reflns_number_total             5123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00052a2.cif
_cod_data_source_block           COMPOUND_5
_cod_depositor_comments
'Adding full bibliography for 7054731--7054734.cif.'
_cod_original_cell_volume        2796.1(5)
_cod_original_formula_sum        'C22.50 H40 Cl2 Ni O3 P2'
_cod_database_code               7054732
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.852
_shelx_res_checksum              90131