####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1921628'
loop_
_audit_author_name
_audit_author_address
'Aleksandr Rubtsov'
;Perm State University
Russia
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-06-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
(10-ethyl-7-phenyl-6,7-dihydro-5H-benzo[b]pyrrolo[1,2-d][1,4]diazepin-5-yl)(phenyl)methanone
_chemical_name_common            ?
_chemical_formula_moiety         C27H24N2O1*H2O
_chemical_formula_sum            'C27 H26 N2 O2'
_chemical_compound_source        'oganic synthesis'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: PE:EA'
_chemical_melting_point          418
_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         410.50

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration ?

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_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.
;

_cell_length_a                   10.4256(14)
_cell_length_b                   12.6372(14)
_cell_length_c                   16.616(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.095(12)
_cell_angle_gamma                90
_cell_volume                     2176.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6619
_cell_measurement_theta_min      3.7770
_cell_measurement_theta_max      29.1940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.079
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.62043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Ruby'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4752
_diffrn_reflns_number            20611
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.224
_diffrn_reflns_theta_max         29.439
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5390
_reflns_number_gt                4160
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1070P)²+0.6963P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5390
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1970
_refine_ls_wR_factor_gt          0.1833
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N7 N 0.44217(15) 0.72590(11) 0.15340(9) 0.0395(3) Uani 1 1 d . . . . .
C10 C 0.47665(17) 0.91557(13) 0.19016(11) 0.0391(4) Uani 1 1 d . . . . .
H10 H 0.388417 0.926059 0.164664 0.047 Uiso 1 1 calc R U . . .
N3 N 0.41160(15) 0.81024(11) 0.30540(9) 0.0408(4) Uani 1 1 d . . . . .
C15 C 0.55554(16) 1.00916(12) 0.16644(10) 0.0354(4) Uani 1 1 d . . . . .
C8 C 0.52342(17) 0.81313(13) 0.15884(10) 0.0376(4) Uani 1 1 d . . . . .
C9 C 0.31735(17) 0.72766(13) 0.17928(11) 0.0395(4) Uani 1 1 d . . . . .
C21 C 0.44402(18) 0.77505(14) 0.38239(11) 0.0419(4) Uani 1 1 d . . . . .
O22 O 0.51132(18) 0.82863(12) 0.43258(9) 0.0646(5) Uani 1 1 d . . . . .
C26 C 0.41560(18) 0.58183(14) 0.35263(11) 0.0423(4) Uani 1 1 d . . . . .
H26 H 0.444551 0.592582 0.302223 0.051 Uiso 1 1 calc R U . . .
C1 C 0.30216(17) 0.76875(13) 0.25566(11) 0.0399(4) Uani 1 1 d . . . . .
C25 C 0.40222(16) 0.66725(13) 0.40365(10) 0.0371(4) Uani 1 1 d . . . . .
C20 C 0.51386(18) 1.06544(14) 0.09711(11) 0.0426(4) Uani 1 1 d . . . . .
H20 H 0.437422 1.045864 0.066781 0.051 Uiso 1 1 calc R U . . .
C5 C 0.5050(2) 0.64001(14) 0.12329(11) 0.0441(4) Uani 1 1 d . . . . .
C11 C 0.18100(19) 0.76976(15) 0.28280(13) 0.0496(5) Uani 1 1 d . . . . .
H11 H 0.170309 0.798225 0.333266 0.060 Uiso 1 1 calc R U . . .
C27 C 0.3861(2) 0.48137(15) 0.37659(12) 0.0481(5) Uani 1 1 d . . . . .
H27 H 0.396094 0.424288 0.342482 0.058 Uiso 1 1 calc R U . . .
C30 C 0.35834(19) 0.64972(15) 0.47817(11) 0.0448(4) Uani 1 1 d . . . . .
H30 H 0.349571 0.706323 0.512934 0.054 Uiso 1 1 calc R U . . .
C16 C 0.66958(18) 1.04087(16) 0.21028(12) 0.0482(5) Uani 1 1 d . . . . .
H16 H 0.700097 1.004193 0.256939 0.058 Uiso 1 1 calc R U . . .
C6 C 0.6358(2) 0.78276(15) 0.13132(12) 0.0478(5) Uani 1 1 d . . . . .
H6 H 0.707773 0.825269 0.127758 0.057 Uiso 1 1 calc R U . . .
C29 C 0.3275(2) 0.54883(16) 0.50130(12) 0.0490(5) Uani 1 1 d . . . . .
H29 H 0.296926 0.537860 0.551216 0.059 Uiso 1 1 calc R U . . .
C18 C 0.6960(2) 1.18056(15) 0.11659(12) 0.0494(5) Uani 1 1 d . . . . .
H18 H 0.742919 1.237670 0.100009 0.059 Uiso 1 1 calc R U . . .
C19 C 0.5835(2) 1.15019(15) 0.07200(12) 0.0498(5) Uani 1 1 d . . . . .
H19 H 0.554238 1.186585 0.024967 0.060 Uiso 1 1 calc R U . . .
C2 C 0.4694(2) 0.91008(15) 0.28178(12) 0.0521(5) Uani 1 1 d . . . . .
H2A H 0.555591 0.916594 0.309711 0.062 Uiso 1 1 calc R U . . .
H2B H 0.418387 0.968915 0.298180 0.062 Uiso 1 1 calc R U . . .
C14 C 0.2107(2) 0.69047(15) 0.13061(13) 0.0506(5) Uani 1 1 d . . . . .
H14 H 0.219489 0.665676 0.078788 0.061 Uiso 1 1 calc R U . . .
C17 C 0.73862(19) 1.12620(17) 0.18569(13) 0.0517(5) Uani 1 1 d . . . . .
H17 H 0.814448 1.146852 0.216194 0.062 Uiso 1 1 calc R U . . .
C28 C 0.34170(19) 0.46470(15) 0.45093(13) 0.0489(5) Uani 1 1 d . . . . .
H28 H 0.321531 0.396648 0.466780 0.059 Uiso 1 1 calc R U . . .
C4 C 0.6238(2) 0.67483(16) 0.10900(13) 0.0526(5) Uani 1 1 d . . . . .
H4 H 0.686888 0.634361 0.087986 0.063 Uiso 1 1 calc R U . . .
C23 C 0.4462(2) 0.53234(15) 0.11484(13) 0.0548(5) Uani 1 1 d . . . . .
H23A H 0.391676 0.528527 0.063869 0.066 Uiso 1 1 calc R U . . .
H23B H 0.391919 0.521564 0.158033 0.066 Uiso 1 1 calc R U . . .
C13 C 0.0903(2) 0.69043(17) 0.15969(16) 0.0603(6) Uani 1 1 d . . . . .
H13 H 0.018990 0.664166 0.127517 0.072 Uiso 1 1 calc R U . . .
C12 C 0.0762(2) 0.72875(17) 0.23531(16) 0.0592(6) Uani 1 1 d . . . . .
H12 H -0.004270 0.727126 0.254686 0.071 Uiso 1 1 calc R U . . .
C24 C 0.5444(3) 0.44502(19) 0.11754(19) 0.0759(7) Uani 1 1 d . . . . .
H24A H 0.608355 0.461949 0.082068 0.114 Uiso 1 1 calc R U . . .
H24B H 0.502466 0.379940 0.100445 0.114 Uiso 1 1 calc R U . . .
H24C H 0.585014 0.437365 0.171833 0.114 Uiso 1 1 calc R U . . .
O31 O 0.6385(4) 1.0217(4) 0.4753(3) 0.1698(14) Uani 1 1 d G . . . .
H31A H 0.597077 0.981320 0.440799 0.255 Uiso 1 1 d G U . . .
H31B H 0.603367 1.020488 0.519159 0.255 Uiso 1 1 d G U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N7 C8 1.387(2) . ?
N7 C5 1.388(2) . ?
N7 C9 1.413(2) . ?
C10 C8 1.496(2) . ?
C10 C15 1.516(2) . ?
C10 C2 1.534(3) . ?
N3 C21 1.363(2) . ?
N3 C1 1.435(2) . ?
N3 C2 1.469(2) . ?
C15 C20 1.384(2) . ?
C15 C16 1.386(3) . ?
C8 C6 1.357(3) . ?
C9 C14 1.386(3) . ?
C9 C1 1.396(3) . ?
C21 O22 1.234(2) . ?
C21 C25 1.484(2) . ?
C26 C27 1.375(3) . ?
C26 C25 1.389(2) . ?
C1 C11 1.386(3) . ?
C25 C30 1.383(2) . ?
C20 C19 1.383(3) . ?
C5 C4 1.359(3) . ?
C5 C23 1.493(3) . ?
C11 C12 1.379(3) . ?
C27 C28 1.381(3) . ?
C30 C29 1.379(3) . ?
C16 C17 1.382(3) . ?
C6 C4 1.416(3) . ?
C29 C28 1.371(3) . ?
C18 C17 1.371(3) . ?
C18 C19 1.373(3) . ?
C14 C13 1.392(3) . ?
C23 C24 1.502(3) . ?
C13 C12 1.369(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
_geom_angle_publ_flag
C8 N7 C5 109.68(15) . . ?
C8 N7 C9 122.90(14) . . ?
C5 N7 C9 127.35(15) . . ?
C8 C10 C15 112.25(13) . . ?
C8 C10 C2 110.99(14) . . ?
C15 C10 C2 112.24(14) . . ?
C21 N3 C1 121.62(14) . . ?
C21 N3 C2 117.59(15) . . ?
C1 N3 C2 118.90(15) . . ?
C20 C15 C16 117.70(16) . . ?
C20 C15 C10 119.08(15) . . ?
C16 C15 C10 123.21(16) . . ?
C6 C8 N7 107.23(15) . . ?
C6 C8 C10 133.37(16) . . ?
N7 C8 C10 119.40(15) . . ?
C14 C9 C1 119.69(18) . . ?
C14 C9 N7 121.65(17) . . ?
C1 C9 N7 118.66(16) . . ?
O22 C21 N3 121.48(16) . . ?
O22 C21 C25 120.20(16) . . ?
N3 C21 C25 118.24(15) . . ?
C27 C26 C25 120.06(17) . . ?
C11 C1 C9 119.65(18) . . ?
C11 C1 N3 120.38(17) . . ?
C9 C1 N3 119.97(16) . . ?
C30 C25 C26 119.10(16) . . ?
C30 C25 C21 119.58(15) . . ?
C26 C25 C21 121.13(15) . . ?
C19 C20 C15 121.36(17) . . ?
C4 C5 N7 106.46(16) . . ?
C4 C5 C23 130.61(18) . . ?
N7 C5 C23 122.85(18) . . ?
C12 C11 C1 120.3(2) . . ?
C26 C27 C28 120.43(17) . . ?
C29 C30 C25 120.44(17) . . ?
C17 C16 C15 120.99(18) . . ?
C8 C6 C4 107.78(17) . . ?
C28 C29 C30 120.21(18) . . ?
C17 C18 C19 119.61(17) . . ?
C18 C19 C20 119.95(18) . . ?
N3 C2 C10 111.64(15) . . ?
C9 C14 C13 119.6(2) . . ?
C18 C17 C16 120.38(19) . . ?
C29 C28 C27 119.75(18) . . ?
C5 C4 C6 108.84(17) . . ?
C5 C23 C24 113.3(2) . . ?
C12 C13 C14 120.5(2) . . ?
C13 C12 C11 120.12(19) . . ?

_refine_diff_density_max         0.332
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.056


