Synthesis and crystallographic characterisation of a homologous series of bis-tridentate phosphine oxide NP3O3 Fe(II), Co(II), Ni(II) and Cu(II) complexes
Page, Samuel J.; Rogers-Simmonds, Daisy; White, Andrew J.P.; Miller, Philip W.; Inorganica Chimica Acta 512 (2020) 119870–; doi:10.1016/j.ica.2020.119870

data_1564091
_publ_section_title
;
 Synthesis and crystallographic characterisation of a homologous series of
 bis-tridentate phosphine oxide NP3O3 Fe(II), Co(II), Ni(II) and Cu(II)
 complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119870
_journal_paper_doi               10.1016/j.ica.2020.119870
_journal_volume                  512
_journal_year                    2020
_chemical_formula_moiety
'C78 H72 Fe N2 O6 P6, 2(C24 H20 B), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C127.5 H115 B2 Cl3 Fe N2 O6 P6'
_chemical_formula_weight         2140.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.896(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8796(7)
_cell_length_b                   18.2086(6)
_cell_length_c                   28.8297(9)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.8650
_cell_measurement_theta_min      2.6450
_cell_volume                     10959.4(6)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19055
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10885
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0326P)^2^+49.9947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6733
_reflns_number_total             10885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119870.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C127.50 H115 B2 Cl3 Fe N2 O6 P6'
_cod_database_code               1564091
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              31766
_shelx_hkl_checksum              44142