Cobalt(ii), iron(ii), zinc(ii) and palladium(ii) complexes of di-topic 4′-{4-[bis(2-pyridyl)aminomethyl]phenyl}-2,2′:6′,2′′-terpyridine. Synthetic and X-ray structural studies
Bray, David J.; Clegg, Jack. K.; Jolliffe, Katrina A.; Lindoy, Leonard F.; CrystEngComm 16 (2014) 6476–; doi:10.1039/c4ce00414k

data_7215865
_publ_section_title
;
 Cobalt(ii), iron(ii), zinc(ii) and palladium(ii) complexes of di-topic
 4&#x2032;-{4-[bis(2-pyridyl)aminomethyl]phenyl}-2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridine.
 Synthetic and X-ray structural studies
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              6476
_journal_paper_doi               10.1039/c4ce00414k
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
;
C64 H49 Fe N12, (H2 O), 1.5(C H4 O), 2.5(Cl O4), 0.5(P F6)
;
_chemical_formula_sum            'C65.5 H57 Cl2.5 F3 Fe N12 O12.5 P0.5'
_chemical_formula_weight         1429.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1075(10)
_cell_length_b                   33.618(4)
_cell_length_c                   11.0207(12)
_cell_measurement_reflns_used    5370
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.37
_cell_measurement_theta_min      2.26
_cell_volume                     3210.1(6)
_computing_cell_refinement       'SAINT (Bruker, 1995)'
_computing_data_collection       'SMART (Bruker, 1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 1995)'
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.0 (CCDC, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'BRUKER SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31618
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.942
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       plate
_exptl_crystal_F_000             1474
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 3346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.047(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         14651
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2357
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                9266
_reflns_number_total             14651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00414k1.cif
_cod_data_source_block           lj243sad
_cod_depositor_comments
'Adding full bibliography for 7215861--7215865.cif.'
_cod_original_cell_volume        3210.2(6)
_cod_original_formula_sum        'C65.50 H57 Cl2.50 F3 Fe N12 O12.50 P0.50'
_cod_database_code               7215865