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_1564090
_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         'C39 H36 N O3 P3, H2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C39 H39 N O5.5 P3'
_chemical_formula_weight         702.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6336(4)
_cell_length_b                   19.7591(7)
_cell_length_c                   26.8567(11)
_cell_measurement_reflns_used    3967
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.8890
_cell_measurement_theta_min      2.9140
_cell_volume                     7234.9(4)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.823
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16332
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_min         2.559
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
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    1.290
_exptl_crystal_description       tablets
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.602
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     593
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0625P)^2^+5.4416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5476
_reflns_number_total             7399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119870.cif
_cod_data_source_block           NP3O3
_cod_original_formula_sum        'C39 H39 N O5.50 P3'
_cod_database_code               1564090
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              8699
_shelx_hkl_checksum              46075