#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:28:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180264 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/50/7115061.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7115061
loop_
_publ_author_name
'Smith, Jeremy M.'
'Lachicotte, Rene J.'
'Holland, Patrick L.'
_publ_section_title
;
 Tuning metal coordination number by ancillary ligand steric effects:
 synthesis of a three-coordinate iron(ii) complex
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1542
_journal_paper_doi               10.1039/b103635c
_journal_year                    2001
_chemical_formula_sum            'C35 H53 Cl Fe N2'
_chemical_formula_weight         593.09
_chemical_melting_point          271.0(10)
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.2370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9014(11)
_cell_length_b                   9.3514(6)
_cell_length_c                   22.7756(15)
_cell_measurement_reflns_used    2132
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     3438.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7361
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red/BrownD
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombic
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0418P)²+2.8195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                2132
_reflns_number_total             2463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103635c.txt
_cod_data_source_block           sad2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '270-272' was changed to '271.0(10)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NA' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115061
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.5000 1.83056(5) 0.7500 0.03331(18) Uani 1 2 d S
Cl1 Cl 0.5000 2.06285(10) 0.7500 0.0688(4) Uani 1 2 d S
N1 N 0.44760(11) 1.69163(19) 0.68667(8) 0.0246(4) Uani 1 1 d .
C1 C 0.41405(14) 1.4376(2) 0.64279(10) 0.0275(5) Uani 1 1 d .
C2 C 0.45486(13) 1.5488(2) 0.69354(10) 0.0236(5) Uani 1 1 d .
C3 C 0.5000 1.4888(3) 0.7500 0.0269(8) Uani 1 2 d S
H3A H 0.5000 1.3872 0.7500 0.032 Uiso 1 2 calc SR
C4 C 0.48206(16) 1.3403(3) 0.63196(11) 0.0378(6) Uani 1 1 d .
H4A H 0.4568 1.2699 0.6000 0.057 Uiso 1 1 calc R
H4B H 0.5107 1.2906 0.6702 0.057 Uiso 1 1 calc R
H4C H 0.5219 1.3986 0.6187 0.057 Uiso 1 1 calc R
C5 C 0.35341(16) 1.3473(3) 0.66629(12) 0.0399(6) Uani 1 1 d .
H5A H 0.3267 1.2760 0.6352 0.060 Uiso 1 1 calc R
H5B H 0.3112 1.4097 0.6742 0.060 Uiso 1 1 calc R
H5C H 0.3839 1.2986 0.7044 0.060 Uiso 1 1 calc R
C6 C 0.36433(16) 1.4955(3) 0.57962(11) 0.0368(6) Uani 1 1 d .
H6A H 0.3420 1.4154 0.5519 0.055 Uiso 1 1 calc R
H6B H 0.4006 1.5532 0.5625 0.055 Uiso 1 1 calc R
H6C H 0.3186 1.5549 0.5840 0.055 Uiso 1 1 calc R
C12 C 0.40984(14) 1.7721(2) 0.63152(10) 0.0270(6) Uani 1 1 d .
C22 C 0.45735(15) 1.8020(2) 0.59140(11) 0.0305(6) Uani 1 1 d .
C32 C 0.42264(17) 1.8904(3) 0.54163(12) 0.0439(7) Uani 1 1 d .
H32A H 0.4529 1.9102 0.5135 0.053 Uiso 1 1 calc R
C42 C 0.34570(18) 1.9502(3) 0.53193(13) 0.0511(8) Uani 1 1 d .
H42A H 0.3231 2.0101 0.4973 0.061 Uiso 1 1 calc R
C52 C 0.30143(17) 1.9229(3) 0.57259(13) 0.0457(7) Uani 1 1 d .
H52A H 0.2483 1.9650 0.5656 0.055 Uiso 1 1 calc R
C62 C 0.33227(15) 1.8357(3) 0.62344(11) 0.0339(6) Uani 1 1 d .
C72 C 0.54393(16) 1.7425(3) 0.60280(11) 0.0381(6) Uani 1 1 d .
H72A H 0.5493 1.6575 0.6303 0.046 Uiso 1 1 calc R
C82 C 0.5633(2) 1.6936(4) 0.54469(14) 0.0606(9) Uani 1 1 d .
H82A H 0.5220 1.6230 0.5231 0.091 Uiso 1 1 calc R
H82B H 0.6186 1.6504 0.5558 0.091 Uiso 1 1 calc R
H82C H 0.5617 1.7761 0.5178 0.091 Uiso 1 1 calc R
C92 C 0.60805(19) 1.8525(4) 0.63630(17) 0.0735(11) Uani 1 1 d .
H92A H 0.5956 1.8839 0.6737 0.110 Uiso 1 1 calc R
H92B H 0.6064 1.9349 0.6094 0.110 Uiso 1 1 calc R
H92C H 0.6633 1.8093 0.6474 0.110 Uiso 1 1 calc R
C102 C 0.28143(17) 1.8109(3) 0.66760(13) 0.0452(7) Uani 1 1 d .
H10A H 0.3159 1.7532 0.7029 0.054 Uiso 1 1 calc R
C112 C 0.2024(2) 1.7269(4) 0.63770(18) 0.0740(11) Uani 1 1 d .
H11A H 0.2165 1.6367 0.6213 0.111 Uiso 1 1 calc R
H11B H 0.1661 1.7834 0.6042 0.111 Uiso 1 1 calc R
H11C H 0.1738 1.7066 0.6684 0.111 Uiso 1 1 calc R
C122 C 0.2597(2) 1.9519(4) 0.69330(15) 0.0640(9) Uani 1 1 d .
H12A H 0.3107 2.0056 0.7125 0.096 Uiso 1 1 calc R
H12B H 0.2312 1.9318 0.7241 0.096 Uiso 1 1 calc R
H12C H 0.2235 2.0085 0.6598 0.096 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 N1 96.35(11) . 2_656
N1 Fe1 Cl1 131.83(5) . .
N1 Fe1 Cl1 131.83(5) 2_656 .
C2 N1 C12 128.38(18) . .
C2 N1 Fe1 124.74(15) . .
C12 N1 Fe1 106.50(13) . .
C6 C1 C5 106.5(2) . .
C6 C1 C4 106.58(19) . .
C5 C1 C4 109.6(2) . .
C6 C1 C2 117.37(19) . .
C5 C1 C2 107.61(18) . .
C4 C1 C2 109.01(19) . .
N1 C2 C3 120.6(2) . .
N1 C2 C1 124.89(19) . .
C3 C2 C1 114.5(2) . .
C2 C3 C2 132.8(3) 2_656 .
C62 C12 C22 121.3(2) . .
C62 C12 N1 119.4(2) . .
C22 C12 N1 118.6(2) . .
C32 C22 C12 117.6(2) . .
C32 C22 C72 120.9(2) . .
C12 C22 C72 121.5(2) . .
C42 C32 C22 121.8(2) . .
C32 C42 C52 119.6(2) . .
C42 C52 C62 121.8(3) . .
C52 C62 C12 117.7(2) . .
C52 C62 C102 119.7(2) . .
C12 C62 C102 122.5(2) . .
C22 C72 C92 110.2(2) . .
C22 C72 C82 114.0(2) . .
C92 C72 C82 109.5(2) . .
C62 C102 C112 112.0(2) . .
C62 C102 C122 111.5(2) . .
C112 C102 C122 109.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9482(18) .
Fe1 N1 1.9482(18) 2_656
Fe1 Cl1 2.1722(11) .
N1 C2 1.346(3) .
N1 C12 1.441(3) .
C1 C6 1.534(3) .
C1 C5 1.541(3) .
C1 C4 1.542(3) .
C1 C2 1.556(3) .
C2 C3 1.403(3) .
C3 C2 1.403(3) 2_656
C12 C62 1.401(3) .
C12 C22 1.412(3) .
C22 C32 1.385(3) .
C22 C72 1.514(3) .
C32 C42 1.372(4) .
C42 C52 1.376(4) .
C52 C62 1.386(4) .
C62 C102 1.522(4) .
C72 C92 1.525(4) .
C72 C82 1.524(4) .
C102 C112 1.525(4) .
C102 C122 1.531(4) .
