#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:19:54 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257353 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/75/1557535.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_1557535
loop_
_publ_author_name
'Bohnenberger, Jan'
'Schmitt, Manuel'
'Feuerstein, Wolfram'
'Krummenacher, Ivo'
'Butschke, Burkhard'
'Czajka, Jakub'
'Malinowski, Przemysław J.'
'Breher, Frank'
'Krossing, Ingo'
_publ_section_title
;
 Completing the triad: synthesis and full characterization of homoleptic
 and heteroleptic carbonyl and nitrosyl complexes of the group VI metals
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              3592
_journal_page_last               3603
_journal_paper_doi               10.1039/C9SC06445A
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C16 Al F36 O4, C5 Mo N O6'
_chemical_formula_sum            'C21 Al F36 Mo N O10'
_chemical_formula_weight         1233.14
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2020-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7152(3)
_cell_length_b                   13.7152(3)
_cell_length_c                   9.5418(3)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.213
_cell_measurement_theta_min      5.201
_cell_volume                     1794.88(8)
_computing_cell_refinement       'SAINT V8.38A (1, 2016)'
_computing_data_collection       'APEX2 v2013..6-2'
_computing_data_reduction        'SAINT V8.38A (1, 2016)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  ShelXle-861
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Smart ApexII Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.106
_diffrn_reflns_theta_min         1.485
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0226
_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)+(0.0310P)²+0.4941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3214
_reflns_number_total             3368
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc06445a2.cif
_cod_data_source_block           p4n_a_CCDC2
_cod_depositor_comments
;Adding full bibliography for 1557531--1557542.cif.

 Adding full bibliography for 1557531--1557542.cif.
;
_cod_original_cell_volume        1794.88(10)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               1557535
_shelx_shelxl_version_number     2016/6
_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+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-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
O1_1 O 0.68486(6) 0.33202(6) 0.10124(10) 0.01646(16) Uani 1 1 d . . . . .
C1_1 C 0.68712(9) 0.41628(8) 0.17460(13) 0.01495(19) Uani 1 1 d . . . . .
C2_1 C 0.58333(9) 0.43368(9) 0.23676(14) 0.0201(2) Uani 1 1 d . . . . .
F1_1 F 0.52207(6) 0.46509(7) 0.13834(10) 0.02754(19) Uani 1 1 d . . . . .
F2_1 F 0.58323(7) 0.49961(7) 0.34004(10) 0.02816(18) Uani 1 1 d . . . . .
F3_1 F 0.54640(7) 0.35116(7) 0.28811(10) 0.0299(2) Uani 1 1 d . . . . .
C3_1 C 0.76130(10) 0.41026(10) 0.29717(14) 0.0224(3) Uani 1 1 d . . . . .
F4_1 F 0.84442(7) 0.37027(8) 0.25397(11) 0.0316(2) Uani 1 1 d . . . . .
F5_1 F 0.72689(8) 0.35590(8) 0.40133(10) 0.0337(2) Uani 1 1 d . . . . .
F6_1 F 0.78316(7) 0.49842(8) 0.35130(10) 0.0307(2) Uani 1 1 d . . . . .
C4_1 C 0.71429(10) 0.50397(10) 0.07877(16) 0.0208(2) Uani 1 1 d . . . . .
F7_1 F 0.81009(7) 0.50756(7) 0.05698(11) 0.0290(2) Uani 1 1 d . . . . .
F8_1 F 0.68776(8) 0.58935(6) 0.13497(10) 0.0304(2) Uani 1 1 d . . . . .
F9_1 F 0.67128(7) 0.49644(7) -0.04561(9) 0.0305(2) Uani 1 1 d . . . . .
Mo1 Mo 0.250000 0.250000 0.37105(2) 0.01768(5) Uani 1 4 d S T P . .
N1 N 0.250000 0.250000 0.1564(3) 0.0273(4) Uani 1 4 d S T P . .
Al1 Al 0.750000 0.250000 0.000000 0.01234(11) Uani 1 4 d S T P . .
O1 O 0.250000 0.250000 0.7085(2) 0.0275(4) Uani 1 4 d S T P . .
C1 C 0.250000 0.250000 0.5909(3) 0.0188(4) Uani 1 4 d S T P . .
O2 O 0.34931(9) 0.46233(8) 0.37103(11) 0.0270(2) Uani 1 1 d . . . . .
C2 C 0.31435(10) 0.38810(10) 0.37123(13) 0.0196(2) Uani 1 1 d . . . . .
O3 O 0.250000 0.250000 0.0380(2) 0.0301(4) Uani 1 4 d S T P . .
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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
_geom_angle_publ_flag
C1_1 O1_1 Al1 146.39(8) . . ?
O1_1 C1_1 C3_1 111.09(10) . . ?
O1_1 C1_1 C4_1 111.23(10) . . ?
C3_1 C1_1 C4_1 109.08(10) . . ?
O1_1 C1_1 C2_1 107.86(10) . . ?
C3_1 C1_1 C2_1 108.64(10) . . ?
C4_1 C1_1 C2_1 108.88(10) . . ?
F1_1 C2_1 F3_1 107.10(11) . . ?
F1_1 C2_1 F2_1 107.48(10) . . ?
F3_1 C2_1 F2_1 107.63(11) . . ?
F1_1 C2_1 C1_1 110.91(11) . . ?
F3_1 C2_1 C1_1 110.87(10) . . ?
F2_1 C2_1 C1_1 112.61(11) . . ?
F5_1 C3_1 F4_1 107.75(11) . . ?
F5_1 C3_1 F6_1 107.19(11) . . ?
F4_1 C3_1 F6_1 107.32(12) . . ?
F5_1 C3_1 C1_1 111.13(11) . . ?
F4_1 C3_1 C1_1 110.49(11) . . ?
F6_1 C3_1 C1_1 112.74(10) . . ?
F9_1 C4_1 F7_1 107.55(13) . . ?
F9_1 C4_1 F8_1 107.76(11) . . ?
F7_1 C4_1 F8_1 107.37(12) . . ?
F9_1 C4_1 C1_1 111.00(11) . . ?
F7_1 C4_1 C1_1 110.90(11) . . ?
F8_1 C4_1 C1_1 112.07(12) . . ?
N1 Mo1 C2 90.04(4) . 2 ?
N1 Mo1 C2 90.04(4) . 4 ?
C2 Mo1 C2 90.0 2 4 ?
N1 Mo1 C2 90.04(4) . 3 ?
C2 Mo1 C2 90.0 2 3 ?
C2 Mo1 C2 179.91(7) 4 3 ?
N1 Mo1 C2 90.05(4) . . ?
C2 Mo1 C2 179.91(7) 2 . ?
C2 Mo1 C2 90.0 4 . ?
C2 Mo1 C2 90.0 3 . ?
N1 Mo1 C1 180.0 . . ?
C2 Mo1 C1 89.96(4) 2 . ?
C2 Mo1 C1 89.96(4) 4 . ?
C2 Mo1 C1 89.96(4) 3 . ?
C2 Mo1 C1 89.95(4) . . ?
O3 N1 Mo1 180.0 . . ?
O1_1 Al1 O1_1 112.16(6) 8_655 7_665 ?
O1_1 Al1 O1_1 108.14(3) 8_655 2_655 ?
O1_1 Al1 O1_1 108.14(3) 7_665 2_655 ?
O1_1 Al1 O1_1 108.15(3) 8_655 . ?
O1_1 Al1 O1_1 108.14(3) 7_665 . ?
O1_1 Al1 O1_1 112.16(6) 2_655 . ?
O1 C1 Mo1 180.0 . . ?
O2 C2 Mo1 179.73(14) . . ?
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
O1_1 C1_1 1.3514(14) . ?
O1_1 Al1 1.7312(9) . ?
C1_1 C3_1 1.5524(18) . ?
C1_1 C4_1 1.5561(18) . ?
C1_1 C2_1 1.5605(17) . ?
C2_1 F1_1 1.3316(16) . ?
C2_1 F3_1 1.3332(16) . ?
C2_1 F2_1 1.3375(15) . ?
C3_1 F5_1 1.3290(17) . ?
C3_1 F4_1 1.3305(16) . ?
C3_1 F6_1 1.3486(16) . ?
C4_1 F9_1 1.3293(17) . ?
C4_1 F7_1 1.3311(17) . ?
C4_1 F8_1 1.3383(16) . ?
Mo1 N1 2.049(3) . ?
Mo1 C2 2.0896(14) 2 ?
Mo1 C2 2.0896(14) 4 ?
Mo1 C2 2.0896(14) 3 ?
Mo1 C2 2.0897(14) . ?
Mo1 C1 2.098(2) . ?
N1 O3 1.129(3) . ?
O1 C1 1.122(3) . ?
O2 C2 1.1252(18) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 O1_1 C1_1 C3_1 -60.79(19) . . . . ?
Al1 O1_1 C1_1 C4_1 60.92(18) . . . . ?
Al1 O1_1 C1_1 C2_1 -179.75(12) . . . . ?
O1_1 C1_1 C2_1 F1_1 -76.16(13) . . . . ?
C3_1 C1_1 C2_1 F1_1 163.33(10) . . . . ?
C4_1 C1_1 C2_1 F1_1 44.65(14) . . . . ?
O1_1 C1_1 C2_1 F3_1 42.70(14) . . . . ?
C3_1 C1_1 C2_1 F3_1 -77.81(13) . . . . ?
C4_1 C1_1 C2_1 F3_1 163.51(11) . . . . ?
O1_1 C1_1 C2_1 F2_1 163.35(11) . . . . ?
C3_1 C1_1 C2_1 F2_1 42.84(14) . . . . ?
C4_1 C1_1 C2_1 F2_1 -75.84(13) . . . . ?
O1_1 C1_1 C3_1 F5_1 -74.66(13) . . . . ?
C4_1 C1_1 C3_1 F5_1 162.38(11) . . . . ?
C2_1 C1_1 C3_1 F5_1 43.83(14) . . . . ?
O1_1 C1_1 C3_1 F4_1 44.89(15) . . . . ?
C4_1 C1_1 C3_1 F4_1 -78.06(13) . . . . ?
C2_1 C1_1 C3_1 F4_1 163.38(11) . . . . ?
O1_1 C1_1 C3_1 F6_1 164.97(11) . . . . ?
C4_1 C1_1 C3_1 F6_1 42.02(15) . . . . ?
C2_1 C1_1 C3_1 F6_1 -76.54(14) . . . . ?
O1_1 C1_1 C4_1 F9_1 39.79(15) . . . . ?
C3_1 C1_1 C4_1 F9_1 162.66(11) . . . . ?
C2_1 C1_1 C4_1 F9_1 -78.94(13) . . . . ?
O1_1 C1_1 C4_1 F7_1 -79.70(14) . . . . ?
C3_1 C1_1 C4_1 F7_1 43.17(15) . . . . ?
C2_1 C1_1 C4_1 F7_1 161.58(11) . . . . ?
O1_1 C1_1 C4_1 F8_1 160.33(11) . . . . ?
C3_1 C1_1 C4_1 F8_1 -76.80(13) . . . . ?
C2_1 C1_1 C4_1 F8_1 41.61(14) . . . . ?
C1_1 O1_1 Al1 O1_1 -157.49(17) . . . 8_655 ?
C1_1 O1_1 Al1 O1_1 -35.81(13) . . . 7_665 ?
C1_1 O1_1 Al1 O1_1 83.35(15) . . . 2_655 ?
