#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:35:22 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224522 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/07/7700790.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_7700790
loop_
_publ_author_name
'Chen, You-Xuan'
'Yang, Hsueh-Hui'
'Lin, Yu-Liang'
'Hou, Ji-Kuan'
'Chu, Yong-Jui'
'Liu, Fu-Chen'
'Lee, Gene-Hsiang'
_publ_section_title
;
 [3 + 2] cycloaddition of azido-bridged molybdenum(ii) complex with
 nitriles and alkynes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12996
_journal_page_last               13005
_journal_paper_doi               10.1039/c9dt02659b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C14 H22 Mo2 N10 O4'
_chemical_formula_weight         586.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-24 deposited with the CCDC.    2019-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.6150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3025(7)
_cell_length_b                   19.3312(12)
_cell_length_c                   10.8564(7)
_cell_measurement_reflns_used    6101
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.24
_cell_volume                     2156.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUEKR SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8326
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.063
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2555
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+1.9468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2396
_reflns_number_total             2555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02659b2.cif
_cod_data_source_block           ic14622
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700790--7700796.cif.
;
_cod_database_code               7700790
_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. 
;
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.812
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
Mo Mo 0.64661(2) 0.41558(2) 0.81370(2) 0.01950(6) Uani 1 1 d . U . . .
N1 N 0.53394(19) 0.5000 0.6861(2) 0.0215(4) Uani 1 2 d S T P . .
N2 N 0.4227(2) 0.5000 0.5981(2) 0.0209(4) Uani 1 2 d S T P . .
N3 N 0.3207(2) 0.5000 0.5158(2) 0.0314(5) Uani 1 2 d S T P . .
N4 N 0.6237(2) 0.5000 0.9494(2) 0.0250(4) Uani 1 2 d S TU P . .
N5 N 0.6657(2) 0.5000 1.0717(2) 0.0269(4) Uani 1 2 d S TU P . .
N6 N 0.7029(3) 0.5000 1.1874(2) 0.0406(6) Uani 1 2 d S T P . .
N7 N 0.7910(2) 0.5000 0.8271(2) 0.0236(4) Uani 1 2 d S T P . .
N8 N 0.8794(2) 0.5000 0.7936(2) 0.0259(4) Uani 1 2 d S T P . .
N9 N 0.9663(2) 0.5000 0.7649(3) 0.0436(6) Uani 1 2 d S T P . .
C1 C 0.65373(17) 0.36302(9) 0.66406(18) 0.0242(3) Uani 1 1 d . U . . .
C2 C 0.49525(17) 0.35664(9) 0.77095(18) 0.0251(3) Uani 1 1 d . U . . .
C3 C 0.6808(2) 0.34341(11) 0.9939(2) 0.0359(5) Uani 1 1 d . . . . .
H3A H 0.6550 0.3611 1.0648 0.043 Uiso 1 1 calc R U . . .
H3B H 0.6619 0.2937 0.9733 0.043 Uiso 1 1 calc R U . . .
C4 C 0.79814(19) 0.36863(10) 0.99554(19) 0.0317(4) Uani 1 1 d . . . . .
H4 H 0.8596 0.3974 1.0720 0.038 Uiso 1 1 calc R U . . .
C5 C 0.82964(18) 0.34569(11) 0.8895(2) 0.0319(4) Uani 1 1 d . . . . .
H5A H 0.8159 0.2960 0.8656 0.038 Uiso 1 1 calc R U . . .
H5B H 0.9091 0.3653 0.8859 0.038 Uiso 1 1 calc R U . . .
O1 O 0.65712(15) 0.33126(7) 0.57529(15) 0.0374(3) Uani 1 1 d . . . . .
O2 O 0.40743(14) 0.31950(8) 0.74178(15) 0.0356(3) Uani 1 1 d . . . . .
N10 N 0.0000 0.64474(11) 0.5000 0.0280(5) Uani 1 2 d S T P . .
C6 C -0.0363(11) 0.6895(7) 0.5904(13) 0.064(4) Uani 0.5 1 d . . P A -1
H6A H -0.1206 0.7114 0.5376 0.096 Uiso 0.5 1 calc R U P A -1
H6B H 0.0301 0.7253 0.6305 0.096 Uiso 0.5 1 calc R U P A -1
H6C H -0.0423 0.6613 0.6626 0.096 Uiso 0.5 1 calc R U P A -1
C7 C 0.108(2) 0.5916(7) 0.553(2) 0.065(3) Uani 0.5 1 d . . P A -1
H7A H 0.0902 0.5593 0.6129 0.097 Uiso 0.5 1 calc R U P A -1
H7B H 0.1909 0.6149 0.6032 0.097 Uiso 0.5 1 calc R U P A -1
H7C H 0.1113 0.5660 0.4765 0.097 Uiso 0.5 1 calc R U P A -1
C8 C -0.0184(11) 0.6856(7) 0.3762(13) 0.055(3) Uani 0.5 1 d . . P A -1
H8A H -0.1078 0.7032 0.3340 0.082 Uiso 0.5 1 calc R U P A -1
H8B H -0.0021 0.6559 0.3118 0.082 Uiso 0.5 1 calc R U P A -1
H8C H 0.0427 0.7246 0.4017 0.082 Uiso 0.5 1 calc R U P A -1
C9 C -0.1200(18) 0.6123(8) 0.439(2) 0.101(6) Uani 0.5 1 d . . P A -1
H9A H -0.1894 0.6470 0.4129 0.151 Uiso 0.5 1 calc R U P A -1
H9B H -0.1301 0.5793 0.5022 0.151 Uiso 0.5 1 calc R U P A -1
H9C H -0.1254 0.5877 0.3576 0.151 Uiso 0.5 1 calc R U P A -1
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'
O O 0.0106 0.0060 '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'
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
C2 Mo C1 80.38(7) . .
C2 Mo N1 93.68(7) . .
C1 Mo N1 94.42(7) . .
C2 Mo C4 104.55(8) . .
C1 Mo C4 104.26(8) . .
N1 Mo C4 155.69(7) . .
C2 Mo N7 167.08(7) . .
C1 Mo N7 98.66(7) . .
N1 Mo N7 73.51(6) . .
C4 Mo N7 88.21(7) . .
C2 Mo N4 104.34(7) . .
C1 Mo N4 165.16(6) . .
N1 Mo N4 71.41(6) . .
C4 Mo N4 88.33(7) . .
N7 Mo N4 73.53(6) . .
C2 Mo C3 70.54(8) . .
C1 Mo C3 110.03(8) . .
N1 Mo C3 147.40(7) . .
C4 Mo C3 36.34(7) . .
N7 Mo C3 121.33(8) . .
N4 Mo C3 84.76(7) . .
C2 Mo C5 108.05(8) . .
C1 Mo C5 69.55(7) . .
N1 Mo C5 149.66(7) . .
C4 Mo C5 36.30(7) . .
N7 Mo C5 83.38(6) . .
N4 Mo C5 120.80(7) . .
C3 Mo C5 62.33(7) . .
N2 N1 Mo 129.54(5) . .
N2 N1 Mo 129.54(5) . 6_565
Mo N1 Mo 97.20(8) . 6_565
N3 N2 N1 179.2(2) . .
N5 N4 Mo 127.59(8) . .
N5 N4 Mo 127.59(8) . 6_565
Mo N4 Mo 91.17(7) . 6_565
N6 N5 N4 178.6(3) . .
N8 N7 Mo 130.49(7) . 6_565
N8 N7 Mo 130.49(7) . .
Mo N7 Mo 91.97(7) 6_565 .
N9 N8 N7 178.3(3) . .
O1 C1 Mo 179.29(16) . .
O2 C2 Mo 176.59(16) . .
C4 C3 Mo 67.90(10) . .
C3 C4 C5 115.97(19) . .
C3 C4 Mo 75.76(11) . .
C5 C4 Mo 76.35(11) . .
C4 C5 Mo 67.35(10) . .
C9 N10 C6 95.5(11) . .
C9 N10 C8 93.8(10) . .
C6 N10 C8 108.1(3) . .
C9 N10 C7 110.2(6) . .
C6 N10 C7 123.0(9) . .
C8 N10 C7 119.3(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo C2 1.9440(18) .
Mo C1 1.9460(18) .
Mo N1 2.1756(13) .
Mo C4 2.1994(18) .
Mo N7 2.2692(14) .
Mo N4 2.2847(14) .
Mo C3 2.3008(19) .
Mo C5 2.3160(18) .
N1 N2 1.222(3) .
N1 Mo 2.1756(13) 6_565
N2 N3 1.127(3) .
N4 N5 1.209(3) .
N4 Mo 2.2847(14) 6_565
N5 N6 1.146(3) .
N7 N8 1.198(3) .
N7 Mo 2.2692(14) 6_565
N8 N9 1.148(3) .
C1 O1 1.157(2) .
C2 O2 1.157(2) .
C3 C4 1.407(3) .
C4 C5 1.411(3) .
N10 C9 1.387(17) .
N10 C6 1.489(13) .
N10 C8 1.498(13) .
N10 C7 1.511(16) .
