#------------------------------------------------------------------------------
#$Date: 2016-08-20 09:26:27 +0300 (Sat, 20 Aug 2016) $
#$Revision: 185922 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/63/7226315.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_7226315
loop_
_publ_author_name
'Panda, Tarun Kanti Kanti'
'Anga, Srinivas'
'Banerjee, Indrani'
'Nayek, Hari Pada'
_publ_section_title
;
 Alkali Metal Complexes Having Sterically Bulky Bis-Iminopyrrolyl Ligands
 -- Control of Dimeric to Monomeric Complex
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA13437H
_journal_year                    2016
_chemical_formula_sum            'C52 H51 N3 O2'
_chemical_formula_weight         749.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3665(4)
_cell_length_b                   17.5179(5)
_cell_length_c                   32.0143(14)
_cell_measurement_reflns_used    10213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.955
_cell_measurement_theta_min      5.049
_cell_volume                     4131.3(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_collection
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies,Version 1.171.35.19 (release 27-10-2011CrysAlis171 .NET)(compiled Oct 27'
_computing_molecular_graphics    'ORTEP III & Olex 2.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            10185
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.955
_diffrn_reflns_theta_min         5.049
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0982P)²+3.4088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2078
_refine_ls_wR_factor_ref         0.2194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3111
_reflns_number_total             3932
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra13437h2.cif
_cod_data_source_block           3-h
_cod_database_code               7226315
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C0AA C 0.4679(4) 0.43125(16) 0.27203(8) 0.0451(7) Uani 1 1 d . U . . .
H0AA H 0.5603 0.4134 0.2892 0.054 Uiso 1 1 calc R U . . .
C1AA C 0.3057(3) 0.46263(15) 0.28491(7) 0.0381(6) Uani 1 1 d . U . . .
C2AA C 0.2307(4) 0.47968(14) 0.32585(8) 0.0394(6) Uani 1 1 d . U . . .
H2AA H 0.2982 0.4713 0.3500 0.047 Uiso 1 1 calc R U . . .
C3AA C -0.0166(3) 0.52649(14) 0.36809(7) 0.0358(6) Uani 1 1 d . U . . .
C4AA C 0.1208(3) 0.54459(14) 0.40297(7) 0.0358(6) Uani 1 1 d . U . . .
C6 C 0.1146(3) 0.50980(15) 0.44206(8) 0.0396(6) Uani 1 1 d . U . . .
H6 H 0.0272 0.4728 0.4475 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2382(4) 0.52988(17) 0.47318(8) 0.0457(7) Uani 1 1 d . U . . .
H7 H 0.2324 0.5061 0.4991 0.055 Uiso 1 1 calc R U . . .
C8 C 0.3684(4) 0.58443(17) 0.46584(9) 0.0476(7) Uani 1 1 d . U . . .
H8 H 0.4495 0.5982 0.4868 0.057 Uiso 1 1 calc R U . . .
C9 C 0.3774(4) 0.61886(15) 0.42670(9) 0.0442(6) Uani 1 1 d . U . . .
H9 H 0.4662 0.6553 0.4213 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2551(3) 0.59925(14) 0.39578(8) 0.0393(6) Uani 1 1 d . U . . .
H10 H 0.2624 0.6228 0.3698 0.047 Uiso 1 1 calc R U . . .
C11 C -0.1410(3) 0.45969(14) 0.38066(8) 0.0364(6) Uani 1 1 d . U . . .
C12 C -0.0959(4) 0.38439(16) 0.37203(10) 0.0489(7) Uani 1 1 d . U . . .
H12 H 0.0088 0.3737 0.3569 0.059 Uiso 1 1 calc R U . . .
C13 C -0.2050(4) 0.32510(17) 0.38570(11) 0.0593(8) Uani 1 1 d . U . . .
H13 H -0.1726 0.2750 0.3796 0.071 Uiso 1 1 calc R U . . .
C14 C -0.3600(4) 0.33911(17) 0.40806(10) 0.0525(7) Uani 1 1 d . U . . .
H14 H -0.4317 0.2989 0.4174 0.063 Uiso 1 1 calc R U . . .
C15 C -0.4085(4) 0.41344(17) 0.41651(9) 0.0467(7) Uani 1 1 d . U . . .
H15 H -0.5145 0.4237 0.4313 0.056 Uiso 1 1 calc R U . . .
C16 C -0.2997(4) 0.47281(15) 0.40306(8) 0.0409(6) Uani 1 1 d . U . . .
H16 H -0.3334 0.5228 0.4091 0.049 Uiso 1 1 calc R U . . .
C17 C -0.1360(3) 0.59669(15) 0.35803(8) 0.0381(6) Uani 1 1 d . U . . .
C18 C -0.1383(4) 0.66283(15) 0.38203(9) 0.0437(6) Uani 1 1 d . U . . .
H18 H -0.0639 0.6663 0.4054 0.052 Uiso 1 1 calc R U . . .
C19 C -0.2495(4) 0.72349(16) 0.37162(10) 0.0525(7) Uani 1 1 d . U . . .
H19 H -0.2472 0.7677 0.3877 0.063 Uiso 1 1 calc R U . . .
C20 C -0.3633(4) 0.71915(18) 0.33776(11) 0.0597(8) Uani 1 1 d . U . . .
H20 H -0.4369 0.7603 0.3307 0.072 Uiso 1 1 calc R U . . .
C21 C -0.3674(4) 0.6526(2) 0.31406(10) 0.0619(9) Uani 1 1 d . U . . .
H21 H -0.4468 0.6484 0.2916 0.074 Uiso 1 1 calc R U . . .
C22 C -0.2538(4) 0.59266(18) 0.32398(9) 0.0503(7) Uani 1 1 d . U . . .
H22 H -0.2557 0.5488 0.3077 0.060 Uiso 1 1 calc R U . . .
N1 N 0.2091(4) 0.48037(17) 0.2500 0.0367(7) Uani 1 2 d S TU P . .
H1 H 0.1021 0.5000 0.2500 0.044 Uiso 1 2 calc R U P . .
N2 N 0.0701(3) 0.50636(12) 0.32780(6) 0.0371(5) Uani 1 1 d . U . . .
O1B O 0.2334(12) 0.6959(4) 0.2436(5) 0.187(5) Uani 0.5 1 d D U P A -1
C2B C 0.1008(13) 0.8140(6) 0.2391(5) 0.129(6) Uani 0.5 1 d D U P A -1
H2BA H 0.1586 0.8555 0.2541 0.154 Uiso 0.5 1 calc R U P A -1
H2BB H 0.0304 0.8350 0.2162 0.154 Uiso 0.5 1 calc R U P A -1
C4B C 0.0835(18) 0.6984(8) 0.2675(6) 0.227(12) Uani 0.5 1 d D U P A -1
H4BA H 0.1167 0.6881 0.2963 0.273 Uiso 0.5 1 calc R U P A -1
H4BB H 0.0003 0.6587 0.2586 0.273 Uiso 0.5 1 calc R U P A -1
C5 C 0.2287(18) 0.7619(7) 0.2246(5) 0.173(7) Uani 0.5 1 d D U P A -1
H5A H 0.2059 0.7529 0.1952 0.207 Uiso 0.5 1 calc R U P A -1
H5B H 0.3478 0.7852 0.2269 0.207 Uiso 0.5 1 calc R U P A -1
C3A C -0.0070(15) 0.7710(6) 0.2653(3) 0.128(4) Uani 0.5 1 d D U P A -1
H3AA H -0.1284 0.7655 0.2540 0.153 Uiso 0.5 1 calc R U P A -1
H3AB H -0.0150 0.7943 0.2928 0.153 Uiso 0.5 1 calc R U P A -1
O2A O 0.6873(9) 0.7500 0.5000 0.079(2) Uani 0.5 2 d S TU P . .
O2B O 1.0187(11) 0.7500 0.5000 0.087(2) Uani 0.5 2 d S TU P . .
C003 C 0.7681(9) 0.6934(3) 0.5143(2) 0.127(2) Uani 1 1 d . U . . .
C004 C 0.9287(10) 0.6911(4) 0.5118(2) 0.133(2) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C1AA C0AA C0AA 107.40(15) . 6_556
C1AA C0AA H0AA 126.3 . .
C0AA C0AA H0AA 126.3 6_556 .
N1 C1AA C0AA 107.4(2) . .
N1 C1AA C2AA 119.7(2) . .
C0AA C1AA C2AA 132.9(2) . .
N2 C2AA C1AA 118.2(2) . .
N2 C2AA H2AA 120.9 . .
C1AA C2AA H2AA 120.9 . .
N2 C3AA C11 107.65(19) . .
N2 C3AA C4AA 113.4(2) . .
C11 C3AA C4AA 110.99(19) . .
N2 C3AA C17 104.67(18) . .
C11 C3AA C17 108.7(2) . .
C4AA C3AA C17 111.2(2) . .
C6 C4AA C10 118.1(2) . .
C6 C4AA C3AA 122.7(2) . .
C10 C4AA C3AA 119.2(2) . .
C4AA C6 C7 120.7(3) . .
C4AA C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C8 C7 C6 120.6(3) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C7 C8 C9 119.2(2) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C10 C9 C8 120.4(3) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C4AA 121.0(2) . .
C9 C10 H10 119.5 . .
C4AA C10 H10 119.5 . .
C12 C11 C16 117.4(2) . .
C12 C11 C3AA 121.8(2) . .
C16 C11 C3AA 120.6(2) . .
C13 C12 C11 120.8(3) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C14 C13 C12 121.0(3) . .
C14 C13 H13 119.5 . .
C12 C13 H13 119.5 . .
C13 C14 C15 119.2(3) . .
C13 C14 H14 120.4 . .
C15 C14 H14 120.4 . .
C14 C15 C16 120.0(3) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 121.6(3) . .
C15 C16 H16 119.2 . .
C11 C16 H16 119.2 . .
C18 C17 C22 117.8(2) . .
C18 C17 C3AA 123.7(2) . .
C22 C17 C3AA 118.5(2) . .
C19 C18 C17 120.9(3) . .
C19 C18 H18 119.5 . .
C17 C18 H18 119.5 . .
C20 C19 C18 120.6(3) . .
C20 C19 H19 119.7 . .
C18 C19 H19 119.7 . .
C19 C20 C21 119.4(3) . .
C19 C20 H20 120.3 . .
C21 C20 H20 120.3 . .
C22 C21 C20 119.9(3) . .
C22 C21 H21 120.0 . .
C20 C21 H21 120.0 . .
C21 C22 C17 121.3(3) . .
C21 C22 H22 119.4 . .
C17 C22 H22 119.4 . .
C1AA N1 C1AA 110.4(3) 6_556 .
C1AA N1 H1 124.8 6_556 .
C1AA N1 H1 124.8 . .
C2AA N2 C3AA 122.0(2) . .
C5 O1B C4B 102.3(8) . .
C3A C2B C5 103.6(9) . .
C3A C2B H2BA 111.0 . .
C5 C2B H2BA 111.1 . .
C3A C2B H2BB 111.0 . .
C5 C2B H2BB 111.0 . .
H2BA C2B H2BB 109.0 . .
O1B C4B C3A 112.5(9) . .
O1B C4B H4BA 109.1 . .
C3A C4B H4BA 109.1 . .
O1B C4B H4BB 109.1 . .
C3A C4B H4BB 109.1 . .
H4BA C4B H4BB 107.8 . .
O1B C5 C2B 116.4(8) . .
O1B C5 H5A 108.2 . .
C2B C5 H5A 108.2 . .
O1B C5 H5B 108.2 . .
C2B C5 H5B 108.2 . .
H5A C5 H5B 107.4 . .
C2B C3A C4B 104.2(9) . .
C2B C3A H3AA 110.9 . .
C4B C3A H3AA 110.9 . .
C2B C3A H3AB 110.9 . .
C4B C3A H3AB 110.9 . .
H3AA C3A H3AB 108.9 . .
C003 O2A C003 122.8(8) . 3_566
C004 O2B C004 117.8(9) 3_566 .
C004 C003 O2A 118.7(7) . .
C003 C004 O2B 120.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C0AA C1AA 1.378(4) .
C0AA C0AA 1.411(5) 6_556
C0AA H0AA 0.9300 .
C1AA N1 1.361(3) .
C1AA C2AA 1.453(3) .
C2AA N2 1.274(3) .
C2AA H2AA 0.9300 .
C3AA N2 1.482(3) .
C3AA C11 1.540(4) .
C3AA C4AA 1.540(3) .
C3AA C17 1.546(3) .
C4AA C6 1.393(3) .
C4AA C10 1.396(4) .
C6 C7 1.395(4) .
C6 H6 0.9300 .
C7 C8 1.374(4) .
C7 H7 0.9300 .
C8 C9 1.392(4) .
C8 H8 0.9300 .
C9 C10 1.382(4) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.388(4) .
C11 C16 1.391(4) .
C12 C13 1.384(4) .
C12 H12 0.9300 .
C13 C14 1.370(4) .
C13 H13 0.9300 .
C14 C15 1.377(4) .
C14 H14 0.9300 .
C15 C16 1.382(4) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C18 1.391(4) .
C17 C22 1.395(4) .
C18 C19 1.383(4) .
C18 H18 0.9300 .
C19 C20 1.372(5) .
C19 H19 0.9300 .
C20 C21 1.392(5) .
C20 H20 0.9300 .
C21 C22 1.379(4) .
C21 H21 0.9300 .
C22 H22 0.9300 .
N1 C1AA 1.361(3) 6_556
N1 H1 0.8600 .
O1B C5 1.307(11) .
O1B C4B 1.344(11) .
C2B C3A 1.380(11) .
C2B C5 1.391(11) .
C2B H2BA 0.9700 .
C2B H2BB 0.9700 .
C4B C3A 1.438(12) .
C4B H4BA 0.9700 .
C4B H4BB 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C3A H3AA 0.9700 .
C3A H3AB 0.9700 .
O2A C003 1.244(6) .
O2A C003 1.244(6) 3_566
O2B C004 1.283(8) 3_566
O2B C004 1.283(8) .
C003 C004 1.187(8) .
