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_1564093
_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 N2 Ni O6 P6, 2(C24 H20 B), 4(C2 H3 N)'
_chemical_formula_sum            'C134 H124 B2 N6 Ni O6 P6'
_chemical_formula_weight         2180.53
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 96.6359(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.47027(12)
_cell_length_b                   19.9660(2)
_cell_length_c                   21.70578(19)
_cell_measurement_reflns_used    8163
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.6500
_cell_measurement_theta_min      3.9580
_cell_volume                     5798.60(9)
_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 0.987
_diffrn_measured_fraction_theta_max 0.951
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19073
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.909
_diffrn_reflns_theta_min         3.303
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.792
_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    1.249
_exptl_crystal_description       needles
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         11172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0438P)^2^+0.7235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9013
_reflns_number_total             11172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-512-119870.cif
_cod_data_source_block           4
_cod_original_cell_volume        5798.59(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564093
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              4918
_shelx_hkl_checksum              14983