A tetradentate metalloligand: synthesis and coordination behaviour of a 2-pyridyl-substituted cyclobutadiene iron complex.
Rezaei Rad, Babak; Herrmann, Dirk; Lescop, Christophe; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4247–4250; doi:10.1039/c3dt52699b

data_7028972
_publ_section_title
;
 A tetradentate metalloligand: synthesis and coordination behaviour of a
 2-pyridyl-substituted cyclobutadiene iron complex.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4247
_journal_page_last               4250
_journal_paper_doi               10.1039/c3dt52699b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C46 H55 Cl2 Fe K N4 O6 Zn'
_chemical_formula_sum            'C46 H55 Cl2 Fe K N4 O6 Zn'
_chemical_formula_weight         991.16
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.918(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4571(2)
_cell_length_b                   16.5968(2)
_cell_length_c                   17.0934(2)
_cell_measurement_reflns_used    12674
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.4430
_cell_measurement_theta_min      3.6980
_cell_volume                     4651.62(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9721
_diffrn_measurement_details
;
  1 omega  -59.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   37.0000 -180.0000 88

  2 omega  -62.00   25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   57.0000  -60.0000 87

  3 omega   31.00   69.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -60.0000 38

  4 omega   77.00  158.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -150.0000 81

  5 omega   84.00  158.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000 -180.0000 74

  6 omega   71.00  102.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  150.0000 31

  7 omega   79.00  154.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -60.0000 75

  8 omega   25.00  106.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   90.0000 81

  9 omega   36.00   69.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -90.0000 33

 10 omega -115.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000   30.0000 103

 11 omega -120.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000 -180.0000 112

 12 omega -162.00 -137.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -66.2458 25

 13 omega   24.00  158.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -15.0000  120.0000 134

 14 omega   23.00  109.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -60.0000 86
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0338806000
_diffrn_orient_matrix_UB_12      0.0708761000
_diffrn_orient_matrix_UB_13      0.0511379000
_diffrn_orient_matrix_UB_21      0.0875083000
_diffrn_orient_matrix_UB_22      -0.0242344000
_diffrn_orient_matrix_UB_23      -0.0156719000
_diffrn_orient_matrix_UB_31      -0.0049931000
_diffrn_orient_matrix_UB_32      0.0548501000
_diffrn_orient_matrix_UB_33      -0.0729119000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27914
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.795
_diffrn_reflns_theta_min         3.719
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0487P)^2^+1.6500P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8008
_reflns_number_total             9169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52699b.txt
_cod_data_source_block           cpd_2
_cod_original_cell_volume        4651.6(1)
_cod_database_code               7028972
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C46 H55 N4 Fe K O6 Zn Cl2'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C)
2.c Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C122(H122), C123(H123),
 C124(H124), C125(H125), C135(H135), C134(H134), C133(H133), C142(H142),
 C143(H143), C144(H144), C145(H145), C132(H132)
;
_shelx_res_checksum              14639
_shelx_hkl_checksum              3570