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_1564094
_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 Cu N2 O6 P6, 2(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C86 H84 B2 Cu F8 N6 O6 P6'
_chemical_formula_weight         1720.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                72.638(7)
_cell_angle_beta                 89.866(6)
_cell_angle_gamma                79.572(6)
_cell_formula_units_Z            1
_cell_length_a                   12.3925(9)
_cell_length_b                   13.0398(10)
_cell_length_c                   13.8009(10)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.0860
_cell_measurement_theta_min      3.5720
_cell_volume                     2090.2(3)
_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 10.4115
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12006
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.785
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.079
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.46 (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    1.367
_exptl_crystal_description       blocks
_exptl_crystal_F_000             891
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7969
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0987P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5191
_reflns_number_total             7969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119870.cif
_cod_data_source_block           5
_cod_database_code               1564094
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              23992
_shelx_hkl_checksum              71400