#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:38:30 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257517 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705278.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_7705278
loop_
_publ_author_name
'Cha, Jeongmin'
'Kwon, Hyunchul'
'Song, Hayoung'
'Lee, Eunsung'
_publ_section_title
;
 Dinitrogen activation by a penta-pyridyl molybdenum complex.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12945
_journal_page_last               12949
_journal_paper_doi               10.1039/d0dt02692a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H25 Mo N7'
_chemical_formula_sum            'C29 H25 Mo N7'
_chemical_formula_weight         567.50
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-10 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.307(3)
_cell_length_b                   11.256(2)
_cell_length_c                   20.349(4)
_cell_measurement_reflns_used    1781
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      2.511
_cell_volume                     3277.0(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       phi-scan
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            3254
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.511
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull violet'
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.963
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0731P)²+38.9779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1706
_reflns_number_total             1781
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02692a2.cif
_cod_data_source_block           cmc21
_cod_depositor_comments
'Adding full bibliography for 7705278--7705279.cif.'
_cod_original_cell_volume        3277.0(12)
_cod_database_code               7705278
_shelx_shelxl_version_number     2016/4
_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.
;
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C10, C6, C4, C2, C1, C5, C9, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C6 \\sim C4 \\sim C2 \\sim C1 \\sim C5 \\sim C9 \\sim C7 \\sim C8:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5) = Uanis(C4)
Uanis(N3) = Uanis(N1)
Uanis(C8) = Uanis(C2)
4. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C2(H2), C9(H9), C7(H7), C8(H8)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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
Mo1 Mo 0.000000 0.50794(5) 0.750000 0.0058(2) Uani 1 4 d S T P . .
N1 N 0.000000 0.6941(5) 0.750000 0.0130(9) Uani 1 4 d S T P . .
N2 N 0.1117(2) 0.5173(3) 0.68162(17) 0.0142(7) Uani 1 1 d . . . . .
N3 N 0.000000 0.3354(5) 0.750000 0.0130(9) Uani 1 4 d S T P . .
C6 C 0.1804(3) 0.6012(4) 0.6894(3) 0.0275(10) Uani 1 1 d . U . . .
C3 C 0.0822(4) 0.7559(5) 0.750000 0.0180(11) Uani 1 2 d S T P . .
N4 N 0.000000 0.2340(7) 0.750000 0.043(3) Uani 1 4 d S T P . .
C10 C 0.1208(3) 0.4400(4) 0.6305(2) 0.0256(9) Uani 1 1 d . U . . .
H10 H 0.074355 0.380359 0.625522 0.031 Uiso 1 1 calc R . . . .
C4 C 0.1738(5) 0.6820(6) 0.750000 0.0370(12) Uani 1 2 d S TU P . .
C1 C 0.000000 0.9403(8) 0.750000 0.041(3) Uani 1 4 d S TU P . .
H1 H 0.000000 1.024710 0.750000 0.049 Uiso 1 4 calc RS T P . .
C2 C 0.0826(7) 0.8795(7) 0.750000 0.0543(13) Uani 1 2 d S TU P . .
H2 H 0.140204 0.921503 0.750000 0.065 Uiso 1 2 calc RS T P . .
C5 C 0.2567(4) 0.7689(6) 0.750000 0.0370(12) Uani 1 2 d S TU P . .
H5A H 0.247249 0.829046 0.784199 0.055 Uiso 0.5 1 calc GR . . A -1
H5B H 0.260992 0.807872 0.707035 0.055 Uiso 0.5 1 calc GR . . A -1
H5C H 0.314609 0.725270 0.758766 0.055 Uiso 0.5 1 calc GR . . A -1
C9 C 0.1919(5) 0.4424(5) 0.5860(3) 0.0503(16) Uani 1 1 d . U . . .
H9 H 0.194255 0.386531 0.551070 0.060 Uiso 1 1 calc R . . . .
C7 C 0.2544(4) 0.6073(5) 0.6451(4) 0.060(2) Uani 1 1 d . U . . .
H7 H 0.300865 0.666665 0.651079 0.072 Uiso 1 1 calc R . . . .
C8 C 0.2624(5) 0.5302(5) 0.5930(4) 0.0543(13) Uani 1 1 d . U . . .
H8 H 0.312939 0.535437 0.562851 0.065 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'
Mo Mo -1.6832 0.6857 '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'
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
N1 Mo1 N2 87.16(8) . . ?
N1 Mo1 N2 87.16(8) . 10_557 ?
N1 Mo1 N2 87.16(8) . 12 ?
N1 Mo1 N2 87.16(8) . 3_556 ?
N2 Mo1 N2 81.99(19) 12 3_556 ?
N2 Mo1 N2 81.99(19) . 10_557 ?
N2 Mo1 N2 97.72(19) . 12 ?
N2 Mo1 N2 174.32(16) 10_557 12 ?
N2 Mo1 N2 97.72(19) 10_557 3_556 ?
N2 Mo1 N2 174.32(16) . 3_556 ?
N3 Mo1 N1 180.0 . . ?
N3 Mo1 N2 92.84(8) . 3_556 ?
N3 Mo1 N2 92.84(8) . . ?
N3 Mo1 N2 92.84(8) . 10_557 ?
N3 Mo1 N2 92.84(8) . 12 ?
C3 N1 Mo1 120.6(3) . . ?
C3 N1 Mo1 120.6(3) 3_556 . ?
C3 N1 C3 118.8(6) 3_556 . ?
C6 N2 Mo1 119.8(3) . . ?
C10 N2 Mo1 122.8(3) . . ?
C10 N2 C6 117.3(4) . . ?
N4 N3 Mo1 180.0 . . ?
N2 C6 C4 117.2(4) . . ?
N2 C6 C7 120.3(5) . . ?
C7 C6 C4 122.5(5) . . ?
N1 C3 C4 117.0(5) . . ?
N1 C3 C2 120.8(6) . . ?
C2 C3 C4 122.2(6) . . ?
N2 C10 H10 117.7 . . ?
C9 C10 N2 124.5(5) . . ?
C9 C10 H10 117.7 . . ?
C6 C4 C6 106.8(5) 10_557 . ?
C6 C4 C3 111.7(3) 10_557 . ?
C6 C4 C3 111.7(3) . . ?
C6 C4 C5 109.3(3) 10_557 . ?
C6 C4 C5 109.3(3) . . ?
C5 C4 C3 108.1(5) . . ?
C2 C1 H1 120.1 3_556 . ?
C2 C1 H1 120.1 . . ?
C2 C1 C2 119.8(10) 3_556 . ?
C3 C2 H2 120.1 . . ?
C1 C2 C3 119.9(8) . . ?
C1 C2 H2 120.1 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C10 C9 H9 120.7 . . ?
C10 C9 C8 118.6(6) . . ?
C8 C9 H9 120.7 . . ?
C6 C7 H7 119.0 . . ?
C8 C7 C6 122.1(6) . . ?
C8 C7 H7 119.0 . . ?
C9 C8 H8 121.4 . . ?
C7 C8 C9 117.2(6) . . ?
C7 C8 H8 121.4 . . ?
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
Mo1 N1 2.096(6) . ?
Mo1 N2 2.121(3) 3_556 ?
Mo1 N2 2.121(3) 10_557 ?
Mo1 N2 2.121(3) 12 ?
Mo1 N2 2.121(3) . ?
Mo1 N3 1.942(6) . ?
N1 C3 1.367(6) 3_556 ?
N1 C3 1.367(6) . ?
N2 C6 1.372(5) . ?
N2 C10 1.362(5) . ?
N3 N4 1.142(10) . ?
C6 C4 1.535(6) . ?
C6 C7 1.393(7) . ?
C3 C4 1.552(9) . ?
C3 C2 1.391(10) . ?
C10 H10 0.9500 . ?
C10 C9 1.362(7) . ?
C4 C6 1.535(6) 10_557 ?
C4 C5 1.537(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.366(11) . ?
C1 C2 1.366(11) 3_556 ?
C2 H2 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C8 1.418(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(10) . ?
C8 H8 0.9500 . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.418 -0.255 0.000 584.0 180.7 ?
2 -0.381 -0.047 0.500 584.0 180.7 ?
