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_7028974
_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
'C8 H16 O2, C34 H31 Cl4 Fe N4 Zn2, C12 H24 K O6'
_chemical_formula_sum            'C54 H71 Cl4 Fe K N4 O8 Zn2'
_chemical_formula_weight         1271.64
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-20
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.168(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8686(8)
_cell_length_b                   14.3500(5)
_cell_length_c                   16.1195(7)
_cell_measurement_reflns_used    4733
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.2670
_cell_measurement_theta_min      3.4650
_cell_volume                     2926.8(3)
_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 0.9927
_diffrn_measured_fraction_theta_max 0.9648
_diffrn_measurement_details
;
  1 omega  -98.00   -2.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000   90.0000 192

  2 omega  -25.00   67.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -37.0000  -90.0000 184

  3 omega   32.00   73.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   30.0000 82

  4 omega   29.00   69.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 80

  5 omega   93.00  154.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 122

  6 omega   77.00  153.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  -60.0000 152

  7 omega   32.00  141.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -150.0000 218

  8 omega   80.00  158.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   90.0000  -31.0000 156

  9 omega   41.00   68.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -30.0000 54

 10 omega   12.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000   60.0000 206

 11 omega   12.00  115.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000 -120.0000 206

 12 omega   46.00  158.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000 -180.0000 224

 13 omega   76.00  158.00   0.5000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 164
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0113926000
_diffrn_orient_matrix_UB_12      -0.0021657000
_diffrn_orient_matrix_UB_13      -0.0991442000
_diffrn_orient_matrix_UB_21      -0.0497018000
_diffrn_orient_matrix_UB_22      0.0979994000
_diffrn_orient_matrix_UB_23      -0.0156038000
_diffrn_orient_matrix_UB_31      0.1105797000
_diffrn_orient_matrix_UB_32      0.0437559000
_diffrn_orient_matrix_UB_33      0.0301101000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15832
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         8.89
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48008
_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 violet'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0654
_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^)+(0.1020P)^2^+6.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                4027
_reflns_number_total             5331
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt52699b.txt
_cod_data_source_block           cpd_4
_cod_original_cell_volume        2926.8(2)
_cod_database_code               7028974
_chemical_oxdiff_formula         'C46 H41 Fe K O6 N4 Zn Cl'
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: O4(0.5) C400(0.5) H11E(0.5) H11F(0.5) C401(0.5) H11H(0.5)
 C402(0.5) H11C(0.5) H11D(0.5) C403(0.5) H11A(0.5) H11B(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) O1(0.67) O2(0.67) O3(0.67) C201(0.67) H10A(0.67) H10B(0.67)
 C202(0.67) H10C(0.67) H10D(0.67) C203(0.67) H10E(0.67) H10F(0.67) C204(0.67)
 H10G(0.67) H10H(0.67) C205(0.67) H10I(0.67) H10J(0.67) C206(0.67) H10K(0.67)
 H10L(0.67) O11(0.33) O12(0.33) O13(0.33) C221(0.33) H12A(0.33) H12B(0.33)
 C222(0.33) H12C(0.33) H12D(0.33) C223(0.33) H12E(0.33) H12F(0.33) C224(0.33)
 H12X(0.33) H12Y(0.33) C225(0.33) H12G(0.33) H12H(0.33) C226(0.33) H12I(0.33)
 H12J(0.33)
 Fixed U12: C3(0) C6(0) Cl1(0) Cl2(0) Cl3(0) Cl4(0) Fe1(0) Zn1(0) Zn2(0) O5(0)
 Fixed U23: C3(0) C6(0) Cl1(0) Cl2(0) Cl3(0) Cl4(0) Fe1(0) Zn1(0) Zn2(0) O5(0)
 Fixed Uiso: H11E(0.103) H11F(0.103) H11G(0.132) H11H(0.132) H11C(0.155)
 H11D(0.155) H11A(0.196) H11B(0.196) H4A(0.081) H4B(0.081) H4C(0.081)
 H5A(0.078) H5B(0.078) H5C(0.078) H6A(0.077) H6B(0.077) H6C(0.077) H72(0.042)
 H73(0.052) H74(0.058) H75(0.046) H82(0.045) H83(0.057) H84(0.054) H85(0.051)
 H10A(0.058) H10B(0.058) H10C(0.103) H10D(0.103) H10E(0.079) H10F(0.079)
 H10G(0.09) H10H(0.09) H10I(0.097) H10J(0.097) H10K(0.069) H10L(0.069)
 H12A(0.061) H12B(0.061) H12C(0.061) H12D(0.061) H12E(0.045) H12F(0.045)
 H12X(0.032) H12Y(0.032) H12G(0.035) H12H(0.035) H12I(0.041) H12J(0.041)
 H20A(0.157) H20B(0.157) H20C(0.152) H20D(0.152)
 Fixed X: H11E(0.1564) H11F(0.0626) H11G(0.1081) H11H(0.1247) H11C(-0.045)
 H11D(-0.0673) H11A(-0.1185) H11B(-0.1025) H4A(0.6763) H4B(0.7635) H4C(0.6703)
 H5A(0.557) H5B(0.4408) H5C(0.5211) H6A(0.3898) H6B(0.3457) H6C(0.4214)
 H72(0.7304) H73(0.8208) H74(0.9903) H75(1.0622) H82(0.7908) H83(0.7157)
 H84(0.5465) H85(0.4664) K1(0) H10A(0.1961) H10B(0.2252) H10C(0.0507)
 H10D(0.0653) H10E(-0.117) H10F(-0.127) H10G(-0.2641) H10H(-0.1958) H10I(-
 0.2876) H10J(-0.3426) H10K(0.3262) H10L(0.2958) H12A(0.3366) H12B(0.2371)
 H12C(0.2462) H12D(0.2326) H12E(0.0779) H12F(0.0862) H12X(-0.0905) H12Y(-
 0.1024) H12G(-0.243) H12H(-0.2308) H12I(-0.3378) H12J(-0.2455) H20A(0.4384)
 H20B(0.3462) H20C(0.555) H20D(0.46)
 Fixed Y: H11E(0.3543) H11F(0.3886) H11G(0.2498) H11H(0.1994) H11C(0.1601)
 H11D(0.2421) H11A(0.3309) H11B(0.2478) C3(0.25) H4A(0.4241) H4B(0.3466)
 H4C(0.3465) H5A(0.4714) H5B(0.4379) H5C(0.4441) C6(0.25) H6A(0.3128)
 H6B(0.2238) H6C(0.2134) H72(0.4722) H73(0.5865) H74(0.5564) H75(0.4132)
 H82(0.4649) H83(0.5935) H84(0.5812) H85(0.4377) Cl1(0.25) Cl2(0.25) Cl3(0.25)
 Cl4(0.25) Fe1(0.25) Zn1(0.25) Zn2(0.25) K1(0.5) H10A(0.5657) H10B(0.6678)
 H10C(0.7092) H10D(0.6615) H10E(0.634) H10F(0.6794) H10G(0.5899) H10H(0.507)
 H10I(0.4156) H10J(0.508) H10K(0.6082) H10L(0.507) H12A(0.6024) H12B(0.6662)
 H12C(0.6207) H12D(0.5158) H12E(0.5217) H12F(0.6296) H12X(0.6504) H12Y(0.5885)
 H12G(0.5192) H12H(0.5889) H12I(0.4562) H12J(0.3874) O5(0.25) H20A(0.3275)
 H20B(0.3275) H20C(0.352) H20D(0.3801)
 Fixed Z: H11E(0.4076) H11F(0.318) H11G(0.2715) H11H(0.3639) H11C(0.2906)
 H11D(0.2196) H11A(0.3023) H11B(0.3699) H4A(1.0752) H4B(1.1101) H4C(1.1414)
 H5A(0.9462) H5B(0.8892) H5C(0.8437) H6A(0.7609) H6B(0.7899) H6C(0.7401)
 H72(0.9247) H73(1.0277) H74(1.1361) H75(1.1389) H82(0.8056) H83(0.7154)
 H84(0.6) H85(0.5714) K1(0.5) H10A(0.3884) H10B(0.4248) H10C(0.3736)
 H10D(0.2922) H10E(0.2266) H10F(0.3108) H10G(0.2472) H10H(0.2382) H10I(0.3177)
 H10J(0.3259) H10K(0.5696) H10L(0.5319) H12A(0.574) H12B(0.5551) H12C(0.4105)
 H12D(0.4329) H12E(0.3012) H12F(0.2889) H12X(0.2954) H12Y(0.2112) H12G(0.2141)
 H12H(0.2928) H12I(0.3009) H12J(0.3105) H20A(0.0496) H20B(0.083) H20C(0.1828)
 H20D(0.2076)
;