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_7028971
_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         'C34 H31 Fe N4'
_chemical_formula_sum            'C34 H31 Fe N4'
_chemical_formula_weight         551.49
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.276(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6884(2)
_cell_length_b                   14.1246(2)
_cell_length_c                   15.0838(2)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.6100
_cell_measurement_theta_min      3.6780
_cell_volume                     2678.99(7)
_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 0.9934
_diffrn_measured_fraction_theta_max 0.9602
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1122087000
_diffrn_orient_matrix_UB_12      -0.0435972000
_diffrn_orient_matrix_UB_13      -0.0441714000
_diffrn_orient_matrix_UB_21      -0.0237251000
_diffrn_orient_matrix_UB_22      0.0570287000
_diffrn_orient_matrix_UB_23      -0.0933224000
_diffrn_orient_matrix_UB_31      0.0431200000
_diffrn_orient_matrix_UB_32      -0.0820420000
_diffrn_orient_matrix_UB_33      -0.0413798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14409
_diffrn_reflns_theta_full        73.68
_diffrn_reflns_theta_max         73.68
_diffrn_reflns_theta_min         3.70
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63391
_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            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0570P)^2^+1.2877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                4952
_reflns_number_total             5200
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt52699b.txt
_cod_data_source_block           cpd_1
_cod_original_cell_volume        2679(1)
_cod_database_code               7028971
_chemical_oxdiff_formula         C34H35FeN4Cu2
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.045) H6B(0.045) H6C(0.045) H7A(0.051) H7B(0.051) H7C(0.051)
 H8A(0.069) H8B(0.069) H8C(0.069) H9A(0.078) H9B(0.078) H9C(0.078) H10A(0.059)
 H10B(0.059) H10C(0.059) H115(0.034) H114(0.033) H113(0.031) H125(0.034)
 H124(0.039) H123(0.038) H135(0.039) H134(0.047) H133(0.045) H145(0.035)
 H144(0.04) H143(0.038) H112(0.027) H122(0.03) H132(0.033) H142(0.031)
 Fixed X: H6A(0.0611) H6B(0.1833) H6C(0.1289) H7A(-0.0565) H7B(-0.024) H7C(-
 0.0718) H8A(0.1361) H8B(0.0687) H8C(0.0223) H9A(0.2848) H9B(0.3186)
 H9C(0.3783) H10A(0.3899) H10B(0.3139) H10C(0.3674) H115(0.5825) H114(0.715)
 H113(0.6883) H125(0.4481) H124(0.3815) H123(0.2725) H135(-0.0582) H134(-
 0.1483) H133(-0.0749) H145(0.0747) H144(0.2132) H143(0.3858) H112(0.5262)
 H122(0.2335) H132(0.0871) H142(0.4124)
 Fixed Y: H6A(0.0622) H6B(0.0423) H6C(0.0423) H7A(0.3013) H7B(0.2043)
 H7C(0.2071) H8A(0.4811) H8B(0.4453) H8C(0.4388) H9A(0.4482) H9B(0.3746)
 H9C(0.3776) H10A(0.2038) H10B(0.1201) H10C(0.1229) H115(0.4561) H114(0.345)
 H113(0.1952) H125(-0.0713) H124(-0.1693) H123(-0.1053) H135(0.0564)
 H134(0.155) H133(0.3013) H145(0.5817) H144(0.6828) H143(0.6224) H112(0.1602)
 H122(0.0555) H132(0.3449) H142(0.4635)
 Fixed Z: H6A(0.3342) H6B(0.3863) H6C(0.2733) H7A(0.3307) H7B(0.3849)
 H7C(0.2718) H8A(0.319) H8B(0.3756) H8C(0.2626) H9A(0.3145) H9B(0.2542)
 H9C(0.3668) H10A(0.3204) H10B(0.2679) H10C(0.3809) H115(0.5225) H114(0.5558)
 H113(0.607) H125(0.5325) H124(0.6163) H123(0.6871) H135(0.5293) H134(0.5915)
 H133(0.6526) H145(0.5468) H144(0.627) H143(0.6921) H112(0.6155) H122(0.669)
 H132(0.6469) H142(0.6687)
;