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_7054734
_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         'C29 H43 Cl Ni O4 P2'
_chemical_formula_sum            'C29 H43 Cl Ni O4 P2'
_chemical_formula_weight         611.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 101.306(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0299(15)
_cell_length_b                   27.236(5)
_cell_length_c                   15.128(3)
_cell_measurement_reflns_used    4374
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.59
_cell_volume                     3244.3(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SHELXTL V 6.12 (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3125
_reflns_number_total             5920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00052a2.cif
_cod_data_source_block           COMPOUND_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Analytical' changed to
'analytical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 7054731--7054734.cif.
;
_cod_original_cell_volume        3244.2(10)
_cod_database_code               7054734
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.961
_exptl_absorpt_special_details
;
The compound display disorder affecting the phenyl ring of the 
benzoate moiety included, which was modeled with SIMU and DELU 
restraints on anisotropic displacement parameters and SAME 
geometrical restraints
;
_shelx_res_checksum              48203