#------------------------------------------------------------------------------
#$Date: 2018-09-08 23:53:01 +0300 (Sat, 08 Sep 2018) $
#$Revision: 210590 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/36/7113624.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_7113624
loop_
_publ_author_name
'MacAdams, Leonard A.'
'Buffone, Gerald P.'
'Incarvito, Christopher D.'
'Golen, James A.'
'Rheingold, Arnold L.'
'Theopold, Klaus H.'
_publ_section_title
;
 A stable alkyl hydride of a first row transition metal
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   10
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1164
_journal_page_last               1165
_journal_paper_doi               10.1039/b301943h
_journal_year                    2003
_chemical_formula_sum            'C42 H52 Cr2 N4'
_chemical_formula_weight         716.88
_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                 92.4850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4971(13)
_cell_length_b                   10.7216(6)
_cell_length_c                   15.0645(9)
_cell_measurement_reflns_used    6307
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.47
_cell_volume                     3791.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11853
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9145
_exptl_absorpt_correction_T_min  0.8882
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.075
_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     221
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0833P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3457
_reflns_number_total             4432
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103661
_cod_data_source_file            b301943h.txt
_cod_data_source_block           jpb13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113624
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
Cr1 Cr 0.228874(14) 0.80839(3) 0.06753(2) 0.02117(14) Uani 1 1 d .
N1 N 0.14925(8) 0.83638(17) 0.10847(13) 0.0219(4) Uani 1 1 d .
N2 N 0.26173(7) 0.90382(17) 0.17398(13) 0.0225(4) Uani 1 1 d .
C1 C 0.10280(9) 0.8238(2) 0.04372(16) 0.0256(5) Uani 1 1 d .
C2 C 0.07495(10) 0.7093(2) 0.03048(18) 0.0315(6) Uani 1 1 d .
C3 C 0.02897(11) 0.7043(3) -0.0300(2) 0.0436(7) Uani 1 1 d .
H3A H 0.0086 0.6282 -0.0378 0.052 Uiso 1 1 calc R
C4 C 0.01192(12) 0.8077(3) -0.0794(2) 0.0505(9) Uani 1 1 d .
H4A H -0.0195 0.8023 -0.1211 0.061 Uiso 1 1 calc R
C5 C 0.04091(11) 0.9180(3) -0.06740(18) 0.0430(7) Uani 1 1 d .
H5A H 0.0294 0.9885 -0.1019 0.052 Uiso 1 1 calc R
C6 C 0.08670(10) 0.9295(3) -0.00601(16) 0.0308(6) Uani 1 1 d .
C7 C 0.13593(9) 0.8705(2) 0.19036(16) 0.0245(5) Uani 1 1 d .
C8 C 0.17568(10) 0.9070(2) 0.25526(16) 0.0279(5) Uani 1 1 d .
H8A H 0.1619 0.9171 0.3132 0.033 Uiso 1 1 calc R
C9 C 0.23404(10) 0.9310(2) 0.24640(16) 0.0263(5) Uani 1 1 d .
C10 C 0.31956(9) 0.9487(2) 0.17072(16) 0.0247(5) Uani 1 1 d .
C11 C 0.36462(10) 0.8759(2) 0.20556(17) 0.0301(6) Uani 1 1 d .
C12 C 0.41925(10) 0.9243(3) 0.20521(19) 0.0362(6) Uani 1 1 d .
H12A H 0.4501 0.8768 0.2301 0.043 Uiso 1 1 calc R
C13 C 0.42983(11) 1.0393(3) 0.16976(19) 0.0412(7) Uani 1 1 d .
H13A H 0.4675 1.0716 0.1710 0.049 Uiso 1 1 calc R
C14 C 0.38531(12) 1.1078(3) 0.1323(2) 0.0400(7) Uani 1 1 d .
H14A H 0.3929 1.1863 0.1061 0.048 Uiso 1 1 calc R
C15 C 0.32964(10) 1.0643(2) 0.13218(17) 0.0306(5) Uani 1 1 d .
C16 C 0.09547(12) 0.5949(3) 0.0793(2) 0.0427(7) Uani 1 1 d .
H16A H 0.0711 0.5239 0.0620 0.064 Uiso 1 1 calc R
H16B H 0.0939 0.6088 0.1434 0.064 Uiso 1 1 calc R
H16C H 0.1348 0.5771 0.0643 0.064 Uiso 1 1 calc R
C17 C 0.11753(12) 1.0506(3) 0.0076(2) 0.0424(7) Uani 1 1 d .
H17A H 0.1006 1.1137 -0.0325 0.064 Uiso 1 1 calc R
H17B H 0.1578 1.0395 -0.0050 0.064 Uiso 1 1 calc R
H17C H 0.1144 1.0779 0.0693 0.064 Uiso 1 1 calc R
C18 C 0.07408(10) 0.8768(3) 0.21412(17) 0.0320(6) Uani 1 1 d .
H18A H 0.0498 0.8488 0.1634 0.048 Uiso 1 1 calc R
H18B H 0.0643 0.9629 0.2291 0.048 Uiso 1 1 calc R
H18C H 0.0680 0.8226 0.2653 0.048 Uiso 1 1 calc R
C19 C 0.26494(11) 0.9957(3) 0.32352(17) 0.0373(6) Uani 1 1 d .
H19A H 0.3050 1.0078 0.3099 0.056 Uiso 1 1 calc R
H19B H 0.2627 0.9443 0.3770 0.056 Uiso 1 1 calc R
H19C H 0.2472 1.0769 0.3336 0.056 Uiso 1 1 calc R
C20 C 0.35450(12) 0.7468(3) 0.2416(2) 0.0443(7) Uani 1 1 d .
H20A H 0.3909 0.7104 0.2627 0.066 Uiso 1 1 calc R
H20B H 0.3373 0.6943 0.1944 0.066 Uiso 1 1 calc R
H20C H 0.3288 0.7520 0.2910 0.066 Uiso 1 1 calc R
C21 C 0.28157(13) 1.1405(3) 0.0917(2) 0.0452(7) Uani 1 1 d .
H21A H 0.2967 1.2181 0.0677 0.068 Uiso 1 1 calc R
H21B H 0.2544 1.1602 0.1373 0.068 Uiso 1 1 calc R
H21C H 0.2622 1.0930 0.0438 0.068 Uiso 1 1 calc R
H1 H 0.2035(12) 0.723(2) -0.0264(18) 0.035(7) Uiso 1 1 d .
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'
Cr Cr 0.3209 0.6236 '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 Cr1 N2 90.55(8) . .
N1 Cr1 Cr1 134.10(6) . 7_565
N2 Cr1 Cr1 135.35(6) . 7_565
N1 Cr1 H1 92.1(9) . .
N2 Cr1 H1 177.3(9) . .
Cr1 Cr1 H1 42.0(9) 7_565 .
C7 N1 C1 116.78(18) . .
C7 N1 Cr1 125.45(15) . .
C1 N1 Cr1 117.72(14) . .
C9 N2 C10 116.78(19) . .
C9 N2 Cr1 125.31(15) . .
C10 N2 Cr1 117.90(15) . .
C6 C1 C2 121.3(2) . .
C6 C1 N1 117.8(2) . .
C2 C1 N1 121.0(2) . .
C3 C2 C1 118.3(3) . .
C3 C2 C16 121.1(2) . .
C1 C2 C16 120.6(2) . .
C2 C3 C4 121.5(3) . .
C2 C3 H3A 119.3 . .
C4 C3 H3A 119.3 . .
C5 C4 C3 119.3(3) . .
C5 C4 H4A 120.4 . .
C3 C4 H4A 120.4 . .
C4 C5 C6 121.8(3) . .
C4 C5 H5A 119.1 . .
C6 C5 H5A 119.1 . .
C5 C6 C1 117.8(3) . .
C5 C6 C17 121.5(3) . .
C1 C6 C17 120.7(2) . .
N1 C7 C8 123.6(2) . .
N1 C7 C18 119.7(2) . .
C8 C7 C18 116.6(2) . .
C7 C8 C9 128.1(2) . .
C7 C8 H8A 115.9 . .
C9 C8 H8A 115.9 . .
N2 C9 C8 123.5(2) . .
N2 C9 C19 119.8(2) . .
C8 C9 C19 116.7(2) . .
C15 C10 C11 120.9(2) . .
C15 C10 N2 119.2(2) . .
C11 C10 N2 120.0(2) . .
C12 C11 C10 118.4(2) . .
C12 C11 C20 120.4(2) . .
C10 C11 C20 121.2(2) . .
C13 C12 C11 121.5(3) . .
C13 C12 H12A 119.2 . .
C11 C12 H12A 119.2 . .
C12 C13 C14 119.4(2) . .
C12 C13 H13A 120.3 . .
C14 C13 H13A 120.3 . .
C13 C14 C15 121.3(3) . .
C13 C14 H14A 119.3 . .
C15 C14 H14A 119.3 . .
C14 C15 C10 118.4(2) . .
C14 C15 C21 120.7(2) . .
C10 C15 C21 121.0(2) . .
C2 C16 H16A 109.5 . .
C2 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C2 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C6 C17 H17A 109.5 . .
C6 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C6 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C7 C18 H18A 109.5 . .
C7 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C7 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C9 C19 H19A 109.5 . .
C9 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C9 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C11 C20 H20A 109.5 . .
C11 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C11 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C15 C21 H21A 109.5 . .
C15 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C15 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N1 2.0178(18) .
Cr1 N2 2.0267(19) .
Cr1 Cr1 2.6206(7) 7_565
Cr1 H1 1.77(3) .
N1 C7 1.337(3) .
N1 C1 1.438(3) .
N2 C9 1.327(3) .
N2 C10 1.444(3) .
C1 C6 1.401(3) .
C1 C2 1.401(3) .
C2 C3 1.384(4) .
C2 C16 1.499(4) .
C3 C4 1.385(4) .
C3 H3A 0.9500 .
C4 C5 1.373(4) .
C4 H4A 0.9500 .
C5 C6 1.394(4) .
C5 H5A 0.9500 .
C6 C17 1.497(4) .
C7 C8 1.379(3) .
C7 C18 1.513(3) .
C8 C9 1.407(3) .
C8 H8A 0.9500 .
C9 C19 1.511(3) .
C10 C15 1.394(3) .
C10 C11 1.399(3) .
C11 C12 1.385(3) .
C11 C20 1.509(4) .
C12 C13 1.371(4) .
C12 H12A 0.9500 .
C13 C14 1.378(4) .
C13 H13A 0.9500 .
C14 C15 1.388(4) .
C14 H14A 0.9500 .
C15 C21 1.502(4) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
