Homoleptic cerium tris(dialkylamido)imidophosphorane guanidinate complexes.
Aguirre Quintana, Luis M.; Jiang, Ningxin; Bacsa, John; La Pierre, Henry S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14908–14913; doi:10.1039/d0dt03472j

data_7705688
_publ_section_title
;
 Homoleptic cerium tris(dialkylamido)imidophosphorane guanidinate
 complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14908
_journal_page_last               14913
_journal_paper_doi               10.1039/d0dt03472j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '(C28 H51 N6 P)2, (C4 H8 O)4, K2'
_chemical_formula_sum            'C72 H136 K2 N12 O4 P2'
_chemical_formula_weight         1374.06
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-12
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.09.11 svn.rc89507dd for OlexSys, GUI svn.r6158)
;
_audit_update_record
;
2020-10-12 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.938(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8786(16)
_cell_length_b                   20.720(2)
_cell_length_c                   22.088(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.77
_cell_measurement_theta_min      2.17
_cell_volume                     7714.6(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61569
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.065
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0967 after correction.
The Ratio of minimum to maximum transmission is 0.6516.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             3008
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.137
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6615
_refine_ls_number_restraints     885
_refine_ls_restrained_S_all      2.703
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.1627
_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/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4009
_refine_ls_wR_factor_ref         0.4197
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.854
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                4853
_reflns_number_total             6615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03472j2.cif
_cod_data_source_block           1-k_sg15
_cod_depositor_comments
'Adding full bibliography for 7705688--7705690.cif.'
_cod_database_code               7705688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.842(3)
 0.158(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 O1_5-C1_5 = O1_5-C4_5
 O1_6-C1_6 = O1_6-C4_6
 O1_8-C1_8 = O1_8-C4_8
 O1_9-C1_9 = O1_9-C4_9
 1.436 with sigma of 0.03
 C2_5-C1_5 = C3_5-C2_5 = C4_5-C3_5
 C2_6-C1_6 = C3_6-C2_6 = C4_6-C3_6
 C2_8-C1_8 = C3_8-C2_8 = C4_8-C3_8
 C2_9-C1_9 = C3_9-C2_9 = C4_9-C3_9
 1.536 with sigma of 0.03
 K1-O1_6 \\sim K1-O1_9
 with sigma of 0.004
 K1-N1_12 \\sim K1-N1_13
 with sigma of 0.02
 K1-O1_5 \\sim K1-O1_8
 with sigma of 0.004
 K1-N1_10 \\sim K1-N1_11
 with sigma of 0.02
 N1_12-C7 \\sim N1_13-C7
 with sigma of 0.002
 N1_13-C7 \\sim N1_10-C7
 with sigma of 0.002
 N1_10-C7 \\sim N1_11-C7
 with sigma of 0.002
 C4_10-C3_10 \\sim C5_10-C4_10
 with sigma of 0.002
 C3_13-C2_13 \\sim C4_13-C3_13
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C1_5) \\sim Ueq, Uanis(C1_6) \\sim Ueq, Uanis(C1_8) \\sim Ueq,
Uanis(C1_9) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2_5) \\sim Ueq, Uanis(C2_6) \\sim Ueq, Uanis(C2_8) \\sim Ueq,
Uanis(C2_9) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C3_5) \\sim Ueq, Uanis(C3_6) \\sim Ueq, Uanis(C3_8) \\sim Ueq,
Uanis(C3_9) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O1_6) = Uanis(O1_9)
Uanis(N1_10) = Uanis(N1_11)
Uanis(C1_12) = Uanis(C2_12) = Uanis(C3_12) = Uanis(C4_12) = Uanis(C5_12) =
Uanis(C6_12) = Uanis(C1_13) = Uanis(C2_13) = Uanis(C3_13) = Uanis(C4_13) =
Uanis(C5_13) = Uanis(C6_13) = Uanis(N1_12) = Uanis(N1_13)
5. Rigid body (RIGU) restrains
 C1_5, C2_5, C3_5, C4_5, O1_5
 C1_6, C2_6, C3_6, C4_6, O1_6
 C1_8, C2_8, C3_8, C4_8, O1_8
 C1_9, C2_9, C3_9, C4_9, O1_9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 N1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10
 N1_11, C1_11, C2_11, C3_11, C4_11, C5_11, C6_11
 N1_12, C1_12, C2_12, C3_12, C4_12, C5_12, C6_12
 N1_13, C1_13, C2_13, C3_13, C4_13, C5_13, C6_13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Same fragment restrains
{N1_11, C1_11, C2_11, C3_11, C4_11, C5_11, C6_11}
{N1_12, C1_12, C2_12, C3_12, C4_12, C5_12, C6_12}
{N1_13, C1_13, C2_13, C3_13, C4_13, C5_13, C6_13}
as
{N1_10, C1_10, C2_10, C3_10, C4_10, C5_10, C6_10} sigma for 1-2: 0.002 1-3:
0.004
{C1_6, C2_6, C3_6, C4_6, O1_6}
{C1_8, C2_8, C3_8, C4_8, O1_8}
{C1_9, C2_9, C3_9, C4_9, O1_9}
as
{C1_5, C2_5, C3_5, C4_5, O1_5} sigma for 1-2: 0.002 1-3: 0.004
7. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) O1(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 O1(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) O1(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) O1(0.5)
 N1(0.5) C1(0.5) H1(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 N1(0.5) C1(0.5) H1(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 N1(0.5) C1(0.5) H1(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 N1(0.5) C1(0.5) H1(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
8.a Ternary CH refined with riding coordinates:
 C1(H1), C1(H1), C1(H1), C1(H1)
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B),
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              61871
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone'
_olex2_submission_special_instructions 'No special instructions were received'