#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:52:35 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294571 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/67/7716744.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_7716744
loop_
_publ_author_name
'Brehm, Philipp C.'
'Schnakenburg, Gregor'
'Streubel, Rainer'
_publ_section_title
;
 Facile synthesis of five-membered cyclic RE₂P-H iron(0)
 complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13201
_journal_page_last               13206
_journal_paper_doi               10.1039/d4dt01313a
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H10 Cl Fe N2 O4 P'
_chemical_formula_sum            'C8 H10 Cl Fe N2 O4 P'
_chemical_formula_weight         320.45
_chemical_name_systematic        PB-107
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.364(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9354(6)
_cell_length_b                   6.4697(10)
_cell_length_c                   14.1938(17)
_cell_measurement_reflns_used    58584
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.89
_cell_volume                     631.62(14)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.795
_diffrn_reflns_theta_min         2.894
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1465 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0189
_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)+(0.0202P)²+0.2385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                3223
_reflns_number_total             3349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01313a2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7716744--7716746.cif.'
_cod_database_code               7716744
_shelx_shelxl_version_number     2017/1
_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   0.837
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, 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
Fe Fe 0.66218(3) 0.29122(5) 0.53869(2) 0.01485(7) Uani 1 1 d . . . . .
Cl Cl 0.63345(7) 0.53834(10) 0.31449(4) 0.02663(13) Uani 1 1 d . . . . .
P P 0.47225(7) 0.41196(9) 0.41757(4) 0.01471(11) Uani 1 1 d . . . . .
O1 O 0.8817(3) 0.0903(3) 0.70365(13) 0.0311(4) Uani 1 1 d . . . . .
O2 O 0.8543(3) 0.6888(3) 0.58524(15) 0.0315(4) Uani 1 1 d . . . . .
O3 O 0.2955(3) 0.2198(3) 0.61585(15) 0.0326(4) Uani 1 1 d . . . . .
O4 O 0.8740(3) 0.0336(3) 0.41578(14) 0.0320(4) Uani 1 1 d . . . . .
N1 N 0.3104(3) 0.5875(3) 0.43249(15) 0.0212(4) Uani 1 1 d . . . . .
N2 N 0.3150(3) 0.2596(3) 0.35361(14) 0.0193(4) Uani 1 1 d . . . . .
C1 C 0.1215(3) 0.5520(4) 0.37691(18) 0.0249(5) Uani 1 1 d . . . . .
H1A H 0.072501 0.680216 0.344128 0.030 Uiso 1 1 calc R . . . .
H1B H 0.025707 0.504608 0.418263 0.030 Uiso 1 1 calc R . . . .
C2 C 0.1559(3) 0.3858(4) 0.30530(17) 0.0235(5) Uani 1 1 d . . . . .
H2A H 0.037489 0.301291 0.288533 0.028 Uiso 1 1 calc R . . . .
H2B H 0.193632 0.448184 0.246655 0.028 Uiso 1 1 calc R . . . .
C3 C 0.3236(4) 0.7463(4) 0.5050(2) 0.0274(5) Uani 1 1 d . . . . .
H3A H 0.460048 0.766761 0.531000 0.041 Uiso 1 1 calc GR . . . .
H3B H 0.249295 0.703697 0.555954 0.041 Uiso 1 1 calc GR . . . .
H3C H 0.270240 0.876009 0.477013 0.041 Uiso 1 1 calc GR . . . .
C4 C 0.3801(4) 0.0916(4) 0.2972(2) 0.0296(6) Uani 1 1 d . . . . .
H4A H 0.480623 0.011572 0.336070 0.044 Uiso 1 1 calc GR . . . .
H4B H 0.433706 0.148798 0.242121 0.044 Uiso 1 1 calc GR . . . .
H4C H 0.269800 0.001493 0.275391 0.044 Uiso 1 1 calc GR . . . .
C5 C 0.7966(4) 0.1674(4) 0.64009(17) 0.0216(5) Uani 1 1 d . . . . .
C6 C 0.7783(3) 0.5359(4) 0.56564(17) 0.0211(5) Uani 1 1 d . . . . .
C7 C 0.4385(3) 0.2444(4) 0.58629(17) 0.0216(5) Uani 1 1 d . . . . .
C8 C 0.7876(3) 0.1323(4) 0.46200(17) 0.0215(5) Uani 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 '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
C5 Fe P 172.89(9) . . ?
C5 Fe C8 89.35(11) . . ?
C6 Fe P 93.53(8) . . ?
C6 Fe C5 92.85(11) . . ?
C6 Fe C7 117.02(11) . . ?
C6 Fe C8 113.22(12) . . ?
C7 Fe P 83.85(8) . . ?
C7 Fe C5 90.45(11) . . ?
C7 Fe C8 129.70(11) . . ?
C8 Fe P 91.02(8) . . ?
Cl P Fe 111.44(3) . . ?
N1 P Fe 120.37(8) . . ?
N1 P Cl 104.74(8) . . ?
N1 P N2 94.00(10) . . ?
N2 P Fe 120.71(8) . . ?
N2 P Cl 102.75(8) . . ?
C1 N1 P 113.94(16) . . ?
C3 N1 P 127.21(17) . . ?
C3 N1 C1 117.8(2) . . ?
C2 N2 P 109.15(15) . . ?
C4 N2 P 121.19(17) . . ?
C4 N2 C2 115.2(2) . . ?
N1 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
N1 C1 C2 105.46(19) . . ?
H1A C1 H1B 108.8 . . ?
C2 C1 H1A 110.6 . . ?
C2 C1 H1B 110.6 . . ?
N2 C2 C1 104.70(19) . . ?
N2 C2 H2A 110.8 . . ?
N2 C2 H2B 110.8 . . ?
C1 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
H2A C2 H2B 108.9 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C5 Fe 179.6(3) . . ?
O2 C6 Fe 178.0(2) . . ?
O3 C7 Fe 178.3(2) . . ?
O4 C8 Fe 177.1(2) . . ?
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
Fe P 2.1726(6) . ?
Fe C5 1.799(2) . ?
Fe C6 1.795(2) . ?
Fe C7 1.796(2) . ?
Fe C8 1.800(3) . ?
Cl P 2.1162(8) . ?
P N1 1.630(2) . ?
P N2 1.653(2) . ?
O1 C5 1.129(3) . ?
O2 C6 1.138(3) . ?
O3 C7 1.136(3) . ?
O4 C8 1.140(3) . ?
N1 C1 1.458(3) . ?
N1 C3 1.449(3) . ?
N2 C2 1.470(3) . ?
N2 C4 1.456(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.519(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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
Fe P N1 C1 -137.11(15) . . . . ?
Fe P N1 C3 30.9(3) . . . . ?
Fe P N2 C2 156.37(13) . . . . ?
Fe P N2 C4 -66.2(2) . . . . ?
Cl P N1 C1 96.57(17) . . . . ?
Cl P N1 C3 -95.4(2) . . . . ?
Cl P N2 C2 -78.85(16) . . . . ?
Cl P N2 C4 58.6(2) . . . . ?
P N1 C1 C2 -13.1(3) . . . . ?
P N2 C2 C1 -37.6(2) . . . . ?
N1 P N2 C2 27.24(17) . . . . ?
N1 P N2 C4 164.7(2) . . . . ?
N1 C1 C2 N2 30.8(2) . . . . ?
N2 P N1 C1 -7.74(19) . . . . ?
N2 P N1 C3 160.3(2) . . . . ?
C3 N1 C1 C2 177.7(2) . . . . ?
C4 N2 C2 C1 -177.9(2) . . . . ?
