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_7028973
_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 Fe2 K N4 O6'
_chemical_formula_sum            'C46 H55 Cl2 Fe2 K N4 O6'
_chemical_formula_weight         981.64
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.109(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4365(9)
_cell_length_b                   16.5146(8)
_cell_length_c                   17.1501(8)
_cell_measurement_reflns_used    7934
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.4010
_cell_measurement_theta_min      3.6950
_cell_volume                     4636.8(4)
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, 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 0.9946
_diffrn_measured_fraction_theta_max 0.9638
_diffrn_measurement_details
;
  1 omega   26.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000 -120.0000 87

  2 omega   39.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000  150.0000 77

  3 omega   92.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000  -90.0000 66

  4 omega   39.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   90.0000 70

  5 omega   87.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -180.0000 71

  6 omega   31.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -90.0000 32

  7 omega   41.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -120.0000 28

  8 omega   31.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 29

  9 omega   88.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   30.0000 70

 10 omega   32.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -60.0000 32

 11 omega   34.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 43

 12 omega  -98.00  -57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000   30.0000 41

 13 omega   12.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000    0.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0562667000
_diffrn_orient_matrix_UB_12      -0.0437746000
_diffrn_orient_matrix_UB_13      0.0629355000
_diffrn_orient_matrix_UB_21      0.0722704000
_diffrn_orient_matrix_UB_22      0.0113639000
_diffrn_orient_matrix_UB_23      -0.0499980000
_diffrn_orient_matrix_UB_31      0.0200718000
_diffrn_orient_matrix_UB_32      0.0814050000
_diffrn_orient_matrix_UB_33      0.0408009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19283
_diffrn_reflns_theta_full        74.18
_diffrn_reflns_theta_max         74.18
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43085
_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            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+1.3049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                7592
_reflns_number_total             9059
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt52699b.txt
_cod_data_source_block           cpd_3
_cod_database_code               7028973
_chemical_oxdiff_formula         'C44 H55 Fe2 N4 K O6 Cl2'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.055) H6B(0.055) H6C(0.055) H7A(0.06) H7B(0.06) H7C(0.06)
 H8A(0.072) H8B(0.072) H8C(0.072) H9A(0.069) H9B(0.069) H9C(0.069) H10A(0.063)
 H10B(0.063) H10C(0.063) H112(0.032) H113(0.035) H114(0.034) H115(0.033)
 H122(0.032) H123(0.036) H124(0.038) H125(0.035) H132(0.033) H133(0.042)
 H134(0.044) H135(0.041) H143(0.052) H144(0.047) H145(0.043) H146(0.033)
 H20A(0.069) H20B(0.069) H20C(0.07) H20D(0.07) H20E(0.079) H20F(0.079)
 H20G(0.08) H20H(0.08) H20I(0.077) H20J(0.077) H20K(0.08) H20L(0.08)
 H20M(0.075) H20N(0.075) H20O(0.074) H20P(0.074) H20Q(0.062) H20R(0.062)
 H20S(0.063) H20T(0.063) H21A(0.063) H21B(0.063) H21C(0.071) H21D(0.071)
 Fixed X: H6A(0.059) H6B(0.0588) H6C(0.1415) H7A(-0.0549) H7B(-0.0633)
 H7C(0.0171) H8A(-0.0688) H8B(-0.0105) H8C(-0.0886) H9A(0.0268) H9B(0.1133)
 H9C(0.0309) H10A(0.1442) H10B(0.1895) H10C(0.1086) H112(0.1472) H113(0.1685)
 H114(0.2721) H115(0.3547) H122(0.2305) H123(0.2916) H124(0.3834) H125(0.4153)
 H132(0.0747) H133(0.072) H134(0.1801) H135(0.2886) H143(0.0083) H144(0.0722)
 H145(0.1859) H146(0.2321) H20A(0.4454) H20B(0.4596) H20C(0.5972) H20D(0.533)
 H20E(0.6252) H20F(0.6943) H20G(0.706) H20H(0.6181) H20I(0.6661) H20J(0.7473)
 H20K(0.821) H20L(0.784) H20M(0.8099) H20N(0.8159) H20O(0.7613) H20P(0.6859)
 H20Q(0.5949) H20R(0.6704) H20S(0.6353) H20T(0.5608) H21A(0.4496) H21B(0.5254)
 H21C(0.418) H21D(0.4232)
 Fixed Y: H6A(0.1777) H6B(0.1269) H6C(0.1364) H7A(0.1015) H7B(0.1485)
 H7C(0.1595) H8A(-0.0212) H8B(-0.0989) H8C(-0.0993) H9A(-0.192) H9B(-0.186)
 H9C(-0.1895) H10A(-0.1034) H10B(-0.0179) H10C(-0.026) H112(0.2008)
 H113(0.3251) H114(0.3382) H115(0.2284) H122(-0.1806) H123(-0.2544) H124(-
 0.1896) H125(-0.0547) H132(-0.0943) H133(-0.2067) H134(-0.2989) H135(-0.2753)
 H143(0.0727) H144(0.1872) H145(0.2375) H146(0.169) H20A(-0.1768) H20B(-0.2707)
 H20C(-0.2567) H20D(-0.2413) H20E(-0.1574) H20F(-0.1666) H20G(-0.0426) H20H(-
 0.0165) H20I(0.0927) H20J(0.0795) H20K(0.0527) H20L(0.1425) H20M(0.1169)
 H20N(0.0201) H20O(0.0629) H20P(0.1034) H20Q(0.0178) H20R(-0.0232) H20S(-
 0.1501) H20T(-0.1146) H21A(-0.1711) H21B(-0.2257) H21C(-0.2321) H21D(-0.1358)
 Fixed Z: H6A(0.0847) H6B(0.0052) H6C(0.0612) H7A(0.2484) H7B(0.1665)
 H7C(0.2253) H8A(0.2759) H8B(0.2851) H8C(0.2223) H9A(0.1764) H9B(0.1406)
 H9C(0.0835) H10A(0.0156) H10B(0.0266) H10C(-0.0321) H112(0.2552) H113(0.1977)
 H114(0.1112) H115(0.093) H122(0.193) H123(0.0987) H124(0.0209) H125(0.0447)
 H132(0.375) H133(0.4569) H134(0.4646) H135(0.3904) H143(0.4869) H144(0.5391)
 H145(0.4801) H146(0.3741) H20A(0.2139) H20B(0.235) H20C(0.2053) H20D(0.1306)
 H20E(0.0714) H20F(0.1431) H20G(0.0742) H20H(0.0997) H20I(0.1875) H20J(0.1436)
 H20K(0.2662) H20L(0.2627) H20M(0.405) H20N(0.4001) H20O(0.517) H20P(0.4653)
 H20Q(0.5258) H20R(0.577) H20S(0.5198) H20T(0.5639) H21A(0.4793) H21B(0.458)
 H21C(0.3575) H21D(0.3464)
;